The Measurement of Total Oxygen in filled BIB wine

The measurement of Total Oxygen
in filled BIB wine
“There shall be one measure of wine throughout our whole realm”
The Magna Carta, 1215
By: Patrick Shea
vitop 
Jean-Claude Vidal
Sophie Vialis
1
Wine BIB O2 measurements / Summary
Part 1: Wine BIB shelf life, by Patrick Shea, Vitop
1.1) Goal
1.2) Key Parameters
1 3) The headspace problem
1.3)
Annex: O2 measurement definitions
Part 2: Measurement technologies,
g , by
y Jean-Claude Vidal,, INRA
2.1) Main measurement technologies
2.2) BIB specificities
P t 3:
Part
3 R
Recommended
d d Procedures,
P
d
by
b Sophie
S hi Vialis,
Vi li Inter-Rhône
I t Rhô
3.1)
3.2)
3.3)
Problems & solutions
Measure Headspace volume
Headspace O2 and DO
Part 4: Future research, by Patrick Shea, Vitop
Photo credits of oxygen sensor instruments and measurements: Marc Maupas, Patrick Shea, Sophie Vialis
2
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Summary
Part 1: Wine BIB shelf life, by Patrick Shea, Vitop
1.1) Goal
1.2) Key Parameters
- Wine
- SO2
- Filtration and sterility
- Oxygen pickup during filling
- Package permeability
- Damage to barrier film
- Storage temperatures
1.3) The headspace problem
Annex: O2 measurement definitions
3
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.1 Goal
Definition of Wine BIB Shelf Life
Length of time before the wine is considered unsuitable for consumption
This is the interval between the filling of the BIB and the last glass consumed
SHELF LIFE GOAL:
Bell curves tightened
(less variance) and/or
shifted
to the right
N° of BIB
Bs
Goal for retailers and fillers: reach or exceed a target (ex: average of 9 months)
while minimizing variance
A
Shelf-life (in months)
4
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.1 Goal
When is BIB wine unacceptable?
•How long can a BIB wine hold up?
This depends upon:
- Changes that occur in the wine (taste, color, etc.)
- A jjudgment
g
that these changes
g are unacceptable
p
The judgment of a BIB wine will be more severe if:
→several conditions must be met to “pass”
p
the test
(for example: free SO2 > 10 mg/l and taste and color acceptable)
→professional tasters are used rather than typical consumers
→compared
co pa ed to
o the
e sa
same
e wine
e in g
glass
ass bo
bottle
e with a sc
screw-cap
e cap
Even when all key shelf-life parameters are mastered:
→a BIB wine may be judged to not last over 9 months if evaluated under severe conditions
→the same wine might be considered acceptable for most wine consumers for up to 12 months
5
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.1 Goal
A special note to importers and retailers
Wine importers and retailers should:
- Fix realistic shelf life requirements (for example 9 months max.) that are adjusted
to the particular wine.
- Adopt good practices (low storage and transport temperatures and quick rotation)
- Be more concerned about helping suppliers meet overall shelf-life goals rather
than fixing performance criteria based upon selected parameters, particularly if
measurement issues are highly complex and non-standardized. Examples of
criteria not to include in specifications: requiring that Dissolved Oxygen (DO) pickup be
<0
0.5
5 mg/L or that the permeability of the bag should be < 0.5
0 5 cm3/m2/day.
/day
- Refer to the Good of Practices for the filling of wine in BIB
6
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.2 Key Parameters
Seven Ways to Extend Wine BIB Shelf
Shelf-Life
Life
It is possible to push forward the limits of shelf life by:
1) Selecting certain types of wines
2) Adding appropriate amounts of SO2
3) Proper final filtration and filling line sterility
4) Minimizing oxygen pickup
y the filling
gp
process
by
5) Selecting a package
with low gas permeability
6) Minimizing damage
to the barrier film
7) Minimizing storage
temperatures
6
9
months
12
7
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.2 Key Parameters
Shelf Life Factor 1: The Wine
Shelf-Life
Expected shelf-life depends upon the specific wine chosen
On the average BIB wines will have a longer shelf life if they:
are red rather than white because reds have more anti-oxidative polyphenols
have high
g alcohol and high
g acid ((low pH)
p )
have a low level of initial dissolved oxygen before bottling
have not already suffered many oxidative reactions
A wine that is oxidized is permanently damaged!
O2
Series of
chemical
reactions
ti
Diminished wine
quality
(aromas, color)
8
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.2 Key Parameters
Shelf Life Factor 2: SO2
Shelf-Life
• SO2 added to wine will contribute to extended shelf-life
• The level of free SO2 upon filling is often 25 to 50 mg/l  this will fall over time
• The
Th id
ideall amountt mustt b
be determined
d t
i d by
b the
th winemaker
i
k and
d will
ill d
depend
d upon:
• “burnt match” odor risk
• Cumulative
C
l ti oxygen ((measured
d or expected)
t d)
• shelf life target
• pH of the wine
• microbiological risks
• other factors
9
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.2 Key Parameters
Shelf Life Factor 2: SO2
Shelf-Life
Example of the fall of Total and Free SO2 for a French Chardonnay in BIB at 20 Ԩ
mg/L
SO2
180
160
Shelf -life
life target = 9 months
140
120
Total SO2
100
Free
ee SO2
80
60
Drop in free
SO2 = 34 mg/L
Initial free SO2 = 46 mg/L
40
20
free SO2 after 9 months = 12 mg/L
0
0
1
2
3
4
5
6
7
months
Source: INRA 2004, Study for Performance BIB
8
9
Note: Minimum free SO2 left to
protect wine from oxidation:
> 10 mg/L
10
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.2 Key Parameters
Shelf Life Factor 3: Microbiological Control
Shelf-Life
Wine BIB shelf-life can be greatly decreased by inadequate final filtration
or lack of sterility during the filling operation
Periodical microbiological analysis + sound hygiene practices can greatly reduce the risk
11
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.2 Key Parameters
Shelf Life Factor 4: O2 Pickup During Filling
Shelf-Life
Important to minimize since 1 extra mg/l of O2 reduces shelf life by one month (INRA
2004)!
Oxygen pickup during filling = ∆ dissolved O2 in the wine + Air cone O2
Air cone O2 is the result of both the volume of the air cone and the % of oxygen inside
•
Key factors to control:
 amount of initial O2 in the empty package
g valve technology
gy
 filling
 filling
g table adjustments
j
 vacuum pack to remove air
 nitrogen flushing of tap and gland to reduce O2
12
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.2 Key Parameters
Shelf Life Factor 5: O2 Permeation of Package
Shelf-Life
Total Life Cycle Package Oxygen (see schema page 22)
= O2 pickup during filling (DO pickup + headspace O2)
+ Filled Package O2 ingress during several months after filling
 Quantify
y the sources of O2 and p
pinpoint
p
potential
p
improvement
p
areas
Through the
tap
Through the
barrier film and
PE film
O2
O2
O2
Through the tap/gland/weld
interfaces
O2
O2
Between the two layers
of welded PE film
O2
Trapped in the
headspace
Trapped in the wine as Dissolved O2
13
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.2 Key Parameters
Shelf Life Factor 6: Damage to Package
Shelf-Life
Damage to the BIB package, particularly to the barrier film, will shorten shelf-life
BIB bags can be examined periodically after filling and after they have gone through the
distribution channels
Flex-cracking
Flex
cracking is normal but if zones of excessive damage are identified
identified, causes should be
determined and corrective action taken
Bag side 1
Metalized polyester BIB bag
examined with back-light
by Gilles Doyon,
Agriculture Canada
Bag side 2
Undamaged zones
Tap
•
It is also important to check the residual space left in
the box ((normallyy + 0.5 litres for a 3 litre box)) since this
can also have an impact on the jiggling of the filled bag
and resulting stress on the film
14
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.2 Key Parameters
Shelf Life Factor 7: Temperature
Shelf-Life
High storage temperatures are the mortal enemy of BIB wines!
Research by the INRA in France has shown that an increase in storage temperature by
10 Ԩ (from 20 Ԩ to 30 Ԩ) will reduce wine BIB shelf-life by half!
This is due to both increased oxygen transmission rates of the package
and to increased rates of chemical reaction in the wine
 Storage and transport temperatures should be maintained under 25 Ԩ
Other research suggests that substantially heating up a filled met-pet BIB bag may
permanently diminish the oxygen barrier of the film
15
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.2 Key Parameters
Who can guarantee wine BIB shelf life?
Should the BIB bag manufacturer
guarantee wine BIB shelf
shelf-life?
life?
No. Because the bag supplier
only controls one of the seven key
parameters that determine shelf
shelf-life
life
Parameter
Who is responsible?
The wine
Winery
SO2
Filler
Microbiological control
Filler
O2 pickup during filling
Filler
Package O2 ingress
Bag manufacturer
Package
g damage
g
Filler/Distributor
Temperature
Filler/Distributor
Should
Sh
ld the
th BIB fill
filler guarantee
t wine
i BIB shelf-life?
h lf lif ?
Partially, but even if the filler also supplies the wine
and buys a quality bag, not all parameters are fully
controllable , since damage to the package
or high temperatures can also occur
after the BIB wines leave the filling centre
16
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.3 The headspace problem
A graphical representation of life cycle O2 management
BIB 3L
17
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.3 The headspace problem
A graphical representation of life cycle O2 management
18
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.3 The headspace problem
A graphical representation of the headspace problem
2O% HS O2
15% HS O2
1O% HS O2
5 % HS O2
19
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / 1.3 The headspace problem
BIB size matters
Potential Headspace oxygen problems become more acute with smaller BIB sizes. The
example below assumes that the size of the air cone (headspace) and DO levels remains
constant as the volume of the BIB package changes. The cone generator line is 6.5 cm and
14.9% air inside is O2. Those packing smaller BIB sizes must manage O2 even better and
retailers pushing for 1
1.5
5 L and 2 L BIB should accept that shelf-life
shelf life is likely to be shortened
shortened.
mg/L O2
Pay special O2
Management
attention to small
capacity BIBs
12
10
8
Headspace Oxygen
DO pick‐up
6
Initial DO
4
2
0
1.5 2
3
5 10 20
Wine volume
of BIB (L) 20
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Annex: O2 definitions
Definitions for keyy terms used in O2 measurements
This Annex can be relevant for measurement definitions referred to relative to
Current Research (part 3 of this presentation)
Dissolved
O
Oxygen
(DO)
in wine
right before
filling
mg/L
Dissolved
Oxygen (DO)
in wine
right
after filling
g
mg/L
O2
O2
+
+
Dissolved
O
Oxygen
(DO)
pickup
during filling
mg/L
Headspace O2
right after filling
in mg/L = (vol
cone ml x % O2 x
1.43 mg/ml)/
(vol vin L)
=
O2
=
Dissolved
O
Oxygen
(DO)
in wine
right
after filling
mg/L
Total Package
Oxygen (TPO)
right
after filling
mg/L
Note: Values surrounded by yellow dashed line are calculated rather than measured.
O2
O2
O2
Key value
to minimize
21
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Annex: O2 definitions
Definitions for keyy terms used in O2 measurements
This Annex can be relevant for measurement definitions referred to relative to
Future Research (part 4 of this presentation)
Total Package
Oxygen (TPO)
right
after filling
mg/L
O2
O2
+
Filled Package
O2 ingress
i
during several
months of
storage mg/L
O2
=
O2
Total Life
Cycle Package
Oxygen during
O2
several months
mg/L
O2
O2
O2
Dissolved
Oxygen (DO)
in wine
right before
filling
mg/L
O2
=
Key value to
minimize
Total Life
C l P
Cycle
Package
k
Oxygen during
O2
several months
mg/L
O2
O2
O2
yg
Total Oxygen
Pickup (TOP)
during
several
months
mg/L
Note: Values surrounded by yellow dashed line are calculated rather than measured.
22
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Annex: O2 definitions
g of the definitions in the remaining
g pages
p g of this
Because of the length
Annex, it is strongly recommended that the reader go directly to Part 2 and
return to this glossary of key terms only if a specific definition is sought.
Volume Definitions
Nominal liquid Volume (L): The volume stated on the label of the package (for example 3L).
Actual liquid volume (L): The true volume of the liquid in the package. For BIB wine, the actual liquid
volume is supposed to be within 1.5% of the nominal liquid volume and the nominal liquid volume is often
used for O2 calculations involving volume, even if this introduces some measurement error.
T t l headspace
h d
l
( L) the
th volume
l
i ) portion
ti off a
Total
volume
(mL):
off th
the gaseous ((air)
closed package space.
Volume capacity of the container (L): For rigid containers (such as glass
bottles), the maximum capacity of the container may be a useful concept but not
for BIB packaging since the maximum capacity of a BIB bag ( i.e. the amount of
gas or liquid that it can hold) is far in excess of its nominal volume and depends
upon the particular manufacturer.
mL
L
Total
T
t l actual
t l volume
l
in
i package
k
(L):
(L) the
th actual
t l liliquid
id volume
l
plus
l h
headspace
d
volume.
23
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Annex: O2 definitions
Pressure and Headspace % O2 Definitions
Partial pressure of oxygen (hPa*): Partial pressure = total pressure x volume fraction of oxygen
component.
p
Each g
gas has a p
partial p
pressure which is the p
pressure which the g
gas would have if it alone
occupied the volume. At 1 bar (=100 kPa = 1000 hPa) and 21% O2, PO2 (the partial pressure of oxygen) = 210 hPa.
Total pressure (hPa): The total pressure of a gas mixture is the sum of the partial pressures of each
individual g
gas in the mixture. In most circumstances atmospheric
p
p
pressure is closely
y approximated
pp
by
y the
hydrostatic pressure caused by the weight of air above the measurement point. Average sea-level
pressure is 1013.25 hPa (1 atm). As elevation increases there is less overlying atmospheric mass, so that
pressure decreases with increasing elevation.
Headspace Oxygen (% O2): % of free molecular oxygen (O2) in the headspace gas. This can also be
expressed as the ratio of the partial pressure of oxygen to total absolute pressure. For measuring
instruments used to compute the % of headspace oxygen in wine packaging, the pressure generally used
for the calculation ((unless an adjustment
j
is made)) is external p
pressure. If it is suspected
p
that the internal
pressure within the package is different than the external pressure, then internal pressure should be
measured and this value should be used for % calculations. For Champagne in a glass bottle the internal
headspace pressure is several times the external pressure but for still wines in bag in box the internal
pressure is g
p
generally
y very
y similar to external p
pressure. Headspace
p
oxygen
yg measurements for BIB
packaging should be taken without applying pressure against the headspace sides during the
measurements since this could introduce some error when the units are expressed in % oxygen.
* Pressure is also often expressed in kPa where 1kPa = 10 hPa
24
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Annex: O2 definitions
Headspace O2 Definitions
Headspace Oxygen (mL O2): The % of headspace oxygen x headspace volume (mL)
Headspace Oxygen (mg O2): Headspace Oxygen (mL O2) x 1.429 mL O2/mg O2
Headspace Oxygen per unit of Total Headspace Volume (mg/L): Headspace Oxygen/Total
H d
Headspace
V
Volume
l
expressed
d iin mg/L
/L
Headspace Oxygen per unit of Nominal Liquid Volume (mg/L) of wine:
Headspace Oxygen/Nominal Liquid Volume expressed in mg/L.
Headspace Oxygen per unit of Actual Liquid Volume (mg/L): Actual volume is
to be preferred over nominal (label) volume if accuracy is sought. The headspace
oxygen
o
yge here
e e ca
can be co
considered
s de ed as a reserve
ese e o
of O2 tthat
at can
ca potentially
pote t a y e
enter
te tthe
e
liquid contained in the package.
O2
25
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Annex: O2 definitions
Dissolved Oxygen (DO) Definitions
DO or Dissolved Oxygen (mg/L): a relative measure of the amount of molecular oxygen (O2) that is
dissolved or carried in a unit volume of a solution . Typically, dissolved oxygen concentrations in wine are
quoted in milligrams per liter (mg/L), where 1 mg/L = 1 part per million (ppm). The maximum amount of
oxygen a wine can contain is around 8 mg/L at 20 Ԩ, which is known as the saturation level. This
saturation level increases with a decrease in temperature.
DO before filling: If used for calculating DO pickup during filling
filling, the DO level just before filling should be
measured for wine in the main storage tank (or at its first exit point). Any other measurement point (during
pumping, hose transport, filtration, buffer tank, etc) is to be considered as partial and should be clearly stated.
DO after filling: DO level right after filling
filling, although
although, depending upon the instrument
used, initial measurements may not be accurate and a stabilization time must be
imposed before the DO value observed more closely reflects the true DO in the wine
DO p
pickup
p during
g filling:
g DO after filling
g - DO before filling
g ((see schema p
page
g 21).
)
This value is the result of both the positive additions of oxygen and the negative
subtractions of oxygen as the wine moves through the entire process from the main
wine tank (via filtration, buffer tank, etc.) to final capping in the filling machine.
Although DO pick-up is generally positive, nitrogen sparging (bubbling nitrogen gas
to remove dissolved oxygen from the wine) or O2 membrane technologies could
potentially result in a negative value.
O2
26
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Annex: O2 definitions
General OTR and Dry Test OTR Definitions
OTR (oxygen transmission rate) the measurement of the amount of oxygen gas that passes through a
material ((component
p
or total p
package)
g ) over a g
given p
period of time.
Dry Test (gas/gas) OTR: measures the amount of oxygen that passes through a material from an
outside atmosphere (generally composed of 20.95% of O2 molecules) into an initially oxygen free
chamber (flushed with nitrogen).
nitrogen) For a “Mocon
Mocon-type
type” test,
test the permeated gas is carried to a detector
which is an extremely sensitive electrical-based sensor capable of detecting minute amounts of oxygen. It
is also possible to use optical or florescence-based gas detection sensors but most cited references for
OTR in BIB packaging are based upon electrical-based sensors. Values in metric units are generally
expressed in cm3 /m2/24 hr.
hr Standard test conditions are often 73 Ԭ (23 Ԩ) and 50% RH but these can be
made to vary.
Correlation between wine BIB shelf-life and Dry Test (gas/gas) OTR results for package components
appears sometimes to be weak in part because the tests are often performed on film before being
transformed into bags and filled but also because true oxygen ingress also depends on many other
factors, including whether liquid is on the other side of the component (the case with BIB) and the surface
contact area. Despite these limits, Dry Test (gas/gas) OTR results are very useful for industrial control
purposes.
27
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Annex: O2 definitions
Filled Package O2 ingress definition
Filled Package O2 ingress* is the measurement of the amount of oxygen (in mg/L)
that p
passes through
g ap
package
g filled with liquid
q
((but also with some headspace
p
air))
during a period (days, weeks months). The outside atmosphere is generally
composed of 20.95% of O2 molecules. Generally the package is filled with high acid
(to keep the micro-organisms at bay), low oxygen water and the change in the level
of dissolved oxygen
yg in the water is observed over many
y weeks or months. Because
of oxygen initially in the headspace or embedded in the package components, a very
long stabilization period (of a least of couple of weeks) is generally observed before
an Oxygen Transmission Rate (OTR) is calculated. Alcohol is sometimes added to
the solution ((when wine is being
g simulated)) but it should be verified that ((for a
particular instrument) the alcohol does not introduce measurement errors.
O2
O2
For Filled Package OTR tests, initial headspace (volume and % O2) can be modified and package
components
t can be
b sealed
l d off
ff (or
( eliminated)
li i t d) to
t see the
th relative
l ti
contribution
t ib ti
off this
thi componentt or
headspace to OTR. Changes in dissolved oxygen (expressed in mg/l or ppm) can be extrapolated to
predict shelf-life but much more work must be done to interpret these curves.
* Referred to also as “Filled Package OTR”
28
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Annex: O2 definitions
TPO and Oxygen pickup during filling definitions
Total Package Oxygen (TPO) is Headspace Oxygen per unit of Actual Liquid Volume (mg/L) + DO in
liquid
q
((mg/L)
g ) at any
y g
given p
point in time,, for example,
p , right
g after filling.
g Please note that the headspace
p
measurement value used is liquid volume rather than headspace volume. Note also that TPO observed
right after filling may not include some oxygen trapped in pockets within the package or film (not yet in the
liquid or headspace).
Dissolved
Oxygen (DO)
in wine
right
after filling
mg/L
O2
+
Headspace O2
right after filling
in mg/L = (vol
cone ml x % O2 x
1.43 mg/ml)/
(vol vin L)
O2
=
Total Package
Oxygen (TPO)
right
after filling
mg/L
O2
O2
Oxygen pickup during filling is Headspace Oxygen per liter of liquid volume (mg/L) + DO pickup (DO
after filling
g - DO before filling)
g) in the liquid
q
((mg/L).
g )
29
Wine BIB O2 measurements / Part 1: Wine BIB shelf life / Annex: O2 definitions
Total Life Cycle Package Oxygen and TOP Definitions
Total Life Cycle Package Oxygen is Total Package Oxygen (TPO) TOP + Filled Package O2 ingress
during
g storage
g of several weeks or months. We did not find a standard expression
p
for this value so this
term has been invented. This value does not take into account the reductive-oxidative history of the wine
before it is measured in the main tank before filling. Performance BIB recommends to minimize Total Life
Cycle Package Oxygen, but if the wine is already nearly oxidized before filling, its shelf-life will not be
veryy long.
g
Total Package
Oxygen (TPO)
right
after filling
g
mg/L
O2
O2
+
Filled Package
O2 ingress
during several
months of
storage mg/L
O2
=
O2
Total Life
Cycle Package
Oxygen during
O2
several months
mg/L
O2
O2
O2
Total Oxygen Pickup (TOP) is the sum of the oxygen pickup during filling (mg/l) + Filled Package O2
ingress during its storage (mg/L). It is also the difference between the Total Life Cycle Package Oxygen
and the dissolved oxygen (DO) in the wine before filling (see schema page 22). This covers a period of
time (extending over many weeks or months) and represents the total amount of oxygen added to a
beverage during the filling process and subsequent storage of the packaged product.
product Filled Package Test
OTR (mg/L) cannot be measured with wine (because it consumes oxygen) so the oxygen pickup after
filling part of TOP must be measured with a water based solution.
30
Wine BIB O2 measurements / Part 2: Measurement technologies / Summary
P t 2:
Part
2 M
Measurementt ttechnologies,
h l i
by Jean-Claude Vidal, INRA
2.1) Main technologies
2.2) BIB specificities
- Viewing headspace volume
- Headspace/wine
H d
/ i ratio
ti
- Rapidity of headspace O2/DO mix
- Package O2 Permeability
- BIB Headspace volume varies over time
- O2 intake once package open
31
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.1 Main technologies
Main Oxygen measurement technologies
There are many technologies used to measure oxygen. An oxygen sensor is an electronic
device that measures the proportion of oxygen in the gas or liquid being analyzed
analyzed.
For filled wine packaging , the two main types of oxygen sensors used are electrodes
(electrochemical sensors) and optodes (optical sensors). This can be used for both oxygen
pickup and oxygen packaging ingress studies.
In addition to these direct measurements of oxygen, it is also possible to indirectly measure
oxygen by measuring color changes in a liquid indicating oxygen ingress
ingress.
Direct O2 measurements
Optodes
Electodes
Indirect O2 measurements
Colorimetric
32
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.1 Main technologies
Colorimetric measure of O2
Several colorimetric methods have been applied to wine bottles, but to our
knowledge none so far to BIB packaging.
knowledge,
packaging These techniques are used for
wine packaging to measure oxygen ingress rather than oxygen pickup
during filling.
- Ribereau-Gayon’s
y
indigo
g carmine method, based on the color
change from the oxidation-reduction reaction of indigo carmine.
- AWRI’s BPAA method using two reagents in a model wine: BPAA
as an oxygen trap and methylene blue and light as a sensitizer.
33
Wine BIB O2 measurements/ Part 2: Measurement technologies/ 2.1 Main technologies
Example of BPAA colorimetric method applied to wine bottle OTR
0.9
0.8
07
0.7
0.6
Dissolved 0.5
O2 (mL) 0.4
0.3
02
0.2
0.1
0
y = 0.005x + 0.401
R2 = 0.99
Oxygen ingress via closure
Oxygen entrapped in closure
coming out and ingress via closure
Oxygen in headspace
and solution
0
20
40
60
80
100
120
Time (days)
Source: Skouroumounis et al (2007) AWITC.
The graph above was presented by Mai Nygaard at the 26 November 2007 Performance BIB meeting in Nîmes
34
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.1 Main technologies
O2 electrodes
The Clark-type electrode is a very commonly used oxygen sensor. Molecular oxygen
passes trough a permeable membrane creating a measurable electrical current and
the intensity of the current rises with a rise in the partial pressure of the oxygen PO2
35
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.1 Main technologies
O2 electrodes  DO
Examples of the measurement of DO in
wine with an electrode.
electrode
BIB
Arrival of liquid
Height =
>1 meter
Circulation chamber
O2 probe
Flowmeter
Measurement
Source:
S
INRA
36
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.1 Main technologies
O2 electrodes  Headspace
Electrodes can also be used to measure headspace oxygen
37
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.1 Main technologies
O2 optodes: How does it work?
Blue light from LED is transmitted through transparent packaging to the surface of sensor
spot where it is absorbed by platinum or ruthenium molecules
spot,
In the absence of oxygen the platinum or ruthenium molecules will emit red light, which is
detected by the optode. The average time between the absorption of the blue light and
the release of the red light allows for the calculation of the oxygen content.
Ruthenium or Platinum
molecules in the Oxygen
sensitive coating of the spot
Blue LED signal
g
sent
through package onto spot
OO22
If excited Ruthenium
or Platinum molecules
transfer energy to O2
mate, then little or no
red fluorescence
signal is sent back to
detector
O2 meter
Box with hardware and
software to calculate
O2 content based
delays of light signals.
If the excited Ruthenium or Platinum
molecules remain alone there is no
energy transfer to O2 molecules and red
light is sent back to detector
O2
Where
are
you?
38
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.1 Main technologies
Optodes
39
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.2 BIB specificities
Bottle headspace easier to see and measure than BIB
40
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.2 BIB specificities
Bottle vs BIB headspace
% of headspace relative to wine volume for bottle and BIB packaging
Wine volume (L)
Headspace
volume (mL)
Bottle
0.75
5
0.7%
9
1,2%
,
Screwcap 14
(Bottle)
65
1.9%
Cork
100
400
BIB
1.5
3
5
4.3% 2.2% 1.3%
6 7% 3.3%
6.7%
3 3% 2.0%
2 0%
26.7% 13.3% 8.0%
10
0.7%
1 0%
1.0%
4.0%
Length of BIB
cone
generator line
6.3 cm
7 4 cm
7.4
12.0 cm
41
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.2 BIB specificities
BIB headspace volume varies over time
Gases that were dissolved (such as CO2) can come out of wine in gas form, adding to
the bubble (air cone) inside the bag.
bag It is thought that after 3 to 5 months the amount of
CO2 permeating from the air cone out through the package will be greater than the CO2
coming out of solution and the size of the air cone will begin to decrease.
Below are the results of the 2004 INRA study for Performance BIB which showed the
headspace volume (mL) in function of storage temperature over a nine month period.
15°C
Headp
Space
(mL)
20°C
25°C
30°C
160
140
120
100
80
60
40
20
0
T0
1 month
3 months
6 months
9 months
42
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.2 BIB specificities
Bottle headspace mixes less rapidly than BIB headspace
O2 in BIB headspace mixes more quickly with the wine because the bag falls more violently
into the box than bottles being placed into boxes on the filling line
line.
43
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.2 BIB specificities
Glass bottles are less permeable to oxygen
Flexible BIB package is more permeable to oxygen than glass as oxygen can enter in
through the film,
film the closure and weld interfaces.
For a glass wine bottle, zero oxygen enters in via the glass and the permeability is
essentially linked to the closure with oxygen going into the wine:
- directly through the closure
- through the closure/glass bottle interface
- which is released from within the closure itself
44
Wine BIB O2 measurements / Part 2: Measurement technologies / 2.2 BIB specificities
Less O2 intake in BIB once opened
As wine is poured from a filled BIB the flexible film collapses around the wine and no air
enters during the pouring process.
process For most BIB taps
taps, closure after use is automatic and
the wine inside will stay fresh for several weeks after opening.
For glass bottles, PET bottles, beverage
cartons and aluminum cans, once the
closure is opened, air enters the package
and shelf
shelf-life
life is considerably reduced
reduced.
Closure after use is manual rather than
automatic.
45
Wine BIB O2 measurements / Part 3: Recommended Procedures / Summary
P t3
Part
3: R
Recommended
d dP
Procedures,
d
by Sophie Vialis, Inter-Rhône
3.1) Problems & solutions
3.2)) Measure Headspace
p
volume
3.3) Headspace O2 and DO
46
Wine BIB O2 measurements/Part 3: Recommended Procedures/3.1 Problems & solutions
The Performance BIB O2 measurement project context
1st problem: For optical measurements, find a better way to maintain the sensor spots
inside the BIB since they come unstuck when glued to flexible PE film
film. It was also important
to avoid introducing a lot of air into the bag while gluing the spot, to avoid making a hole in
the bag (when fixing a viewing window, for example) and to keep as close to realistic fill
conditions as possible.
Solution: Use of a transparent Vitop tap with spot glued inside tap to measure wine or
headspace oxygen after filling the BIB.
47
Wine BIB O2 measurements/Part 3: Recommended Procedures/3.1 Problems & solutions
The Performance BIB O2 measurement project context
2nd problem: Standardize O2 measurement protocol after filling
Solution: Conduct both lab and field tests and suggest protocol based upon experience
48
Wine BIB O2 measurements/Part 3: Recommended Procedures/3.1 Problems & solutions
The Performance BIB O2 measurement project context
3rd problem: Increase the precision and simplicity of the the measurement of headspace
volume
Solution: Creation of the Bib Cone Meter
49
Wine BIB O2 measurements / Part 3: Recommended Procedures / 3.2 Headspace volume
The birth of the BIB cone meter
1st stage: Determination of the true angle of the air cone in a filled BIB package
This was done by developing a protoype cone meter that exactly fit the angle created by the
two sides and then measuring the angle with a protractor. This was further verified
mathematically The true angle is very close to 56°
mathematically.
56
B
C
A
If AB = 5.3, CB = 6 and angle b = 90° then
angle y = 27
27.95
95° and
95°
α = 2 y = 55.90°
55.90°
50
Wine BIB O2 measurements / Part 3: Recommended Procedures / 3.2 Headspace volume
The birth of the BIB cone meter
2nd stage: Determination of the relationship between the length of the cone
generator line and the volume of the air cone (headspace)
This was done by adding a pre-determined quantity of liquid into the bag (for example 50
mL) and reading out the length of the side of the cone generator line (for example 5
5.75
75 cm)
for a wide range of liquid volumes. This was repeated for several nominal volumes.
51
Wine BIB O2 measurements / Part 3: Recommended Procedures / 3.2 Headspace volume
The birth of the BIB cone meter
3rd stage: Establishing a power equation to express the correlation
Volume (mL)
Thi was done
This
d
on the
th b
basis
i off allll th
the reall results
lt gathered
th d iin stage
t
2
120
110
100
90
80
70
60
50
40
30
20
10
0
y = 0.363x2.816
R² = 0.999
moyennes des 5 mesures
Average of 5 results
points initiaux
All results
0
2
4
6
8
for each volume
for each volume
10
Length of cone generator line (cm)
4th stage: Setting an upper limit: 12 cm max. (almost 400 mL of air!)
52
Wine BIB O2 measurements / Part 3: Recommended Procedures / 3.2 Headspace volume
The birth of the BIB cone meter
5th stage: Validation of BIB bags of
different nominal volumes (1.5
(1 5 to 20L) with
bags from several different manufacturers.
6th stage: Printing of the BIB Cone Meter on
a plastic support (about the thickness of a credit
card).
53
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
At what points are oxygen pickup measured?
Oxygen pickup is measured between two points in the filling process
We suggest that BIB wine O2 pickup during filling be defined as the difference between the Total Package
Oxygen (TPO) of the filled BIB (very close to the filler) and the initial DO of the wine in the main tank (or
close to it).
Other points in-between (before and after filtration, exit buffer tank, entry filler, BIB still held by gripper
ja s of filling machine etc
jaws
etc.)) ma
may help identif
identify pick
pickup
p sources
so rces b
butt these represent only
onl partial pick
pickup
p
points. It is important to agree on terms!
54
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Be prepared
It is preferable to use transparent bags for O2 tests since visual control of headspace is
much easier with transparent bags.
bags For both optical and electrochemical measurements,
measurements the
winery should refer to the user manual for guidance. For optical measurements it is also
recommended to:
- Use a transparent tap as a support for the sensor spot and preferably a tap which
has been modified so that it can be removed from its gland after the measurement
has been taken and used (with its glued spot) for other tests.
- Verify that the sensor spots have not exceeded their date or use limits.
- Glue
Gl th
the sensor spott severall hours
h
b f
before
use, choosing
h
i a place
l
on th
the inside
i id
of the tap which is accessible (from the outside of the tap) by the optical cable.
- Store the spots (or taps with spots) away from light.
light
Test wine bags should be clearly identified as not for commercial use.
55
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Calibration
For all O2 measurement technologies, proper calibration is recommended to increase precision.
For optical technologies, there are two sources of obtaining calibration values:
First option is to use the values supplied by the manufacturer for each lot of sensor spots
delivered.
Second option is for the user to perform calibration, taking into account local conditions to
increase
c ease p
precision.
ec s o
The values for the first option are determined under the laboratory conditions of the manufacturer (not
taking into account the aging of the spots, the support upon which it is glued, the length of the optical
cable used,
used etc.).
etc ) A calibration by the user allows for an adjustment to these local conditions
conditions.
It is good practice to maintain a traceability of spots (and taps having specific spots glued to them) and
their calibration values, and to enter their right calibration values for each new test with an optical
instrument.
56
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Calibration
Calibration is performed generally with two points: for example at 0 % oxygen (low point)
and 21% oxygen v/v (high point)
point).
The user can either apply the instructions of the manufacturer or develop their own
calibration method. The easiest ((for the low point)
p
) is to create 0%
% O2 in a small chamber
which can be in part the tap itself, held open (for nitrogen flushing) by a connector.
57
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Initial DO measurements in the main wine tank*
tank
There are three main sampling techniques:
-Inside the tank: A dipping probe can be fed into the tank from above, with measurements at the bottom,
the top and the middle of the tank to test homogenity and to obtain an average value.
- At the tank main exit: For optodes,
optodes a sensor spot can be glued on a transparent glass window one one
of the connection links at the exit of the wine tank. If a glass window is used, it should be transparent and
not too thick (< 12 mm). If the wine is too cold, condensation on the glass can prevent the correct
measurement from being taken. Some optodes (with integrated sensor spots) require a liquid circulation
chamber connected to the exit of the main wine tank
tank.
For electrodes, wine can be drawn into the instrument (from a deviation link placed in the exit hose) and
measured.
- Draw a sample from the tasting tap. For optodes, the wine can be placed in a small glass recipient
(fushed previously with inert gas) with a sensor spot. This method is not recommended if other options
are available. For electrodes, the measurement can be taken by directly making the wine flow from the
tasting tap.
* By main wine tank, we mean the main tank used for filling, before final filtration and any buffer tank.
58
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Initial DO measurements directly
into the main wine tank
The in-tank dipping method for opical measurements: Dipping probe fed into the tank
from above or via a side tank (shown). It is best to stir the probe while it is the tank to
decrease stabilisation time.
59
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Initial DO measurements exit from the main wine tank
This can be conducted directly at the exit of the main wine tank with an optical instrument.
For some optical technologies
technologies, a sopt can be glued on the other side of a transparent
window to allow this measurement to take place..
60
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Initial DO measurements exit from the main wine tank
Results from several measurement technologies can be compared at the same point of exit.
2 optodes
Transparent
window with
spots for
optical
measurements
Flow unit for
electrochemical
method
th d
Circulation chamber for optical
measurement with integrated spot
61
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
TPO measurements after filling
For all measurement technologies it is not easy to take the first measurement (after filling
and capping) while the wine BIB is still held by the grippers of the filling machine
machine.
For this reason it is recommended to take the BIB
sample right after it has been filled and tapped but
to gently catch it as soon as it is released by the
grippers but before the bag has fallen into the box.
This generally implies that the machine must be
temporarily stopped when the sample is taken
taken.
When the BIB is taken, it should be gently
transported
p
(holding
(
g the tap
p on top)
p) to a test table
located close to the filling machine. The BIB should be
readied first for headspace analysis (for optical
measurements) without mixing the wine.
62
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
TPO measurements after filling
Because the same sensor spot can be used for headspace oxygen and for DO (by
reversing the position of the BIB)
BIB), there is a need for only one BIB for each optical sample
set.
63
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Measuring headspace volume
- Prepare an ample work space with cone meter
- For optodes: calculate headspace volume right after headspace oxygen has been
measured and just before the DO measurements for the wine.
-For electrodes: measure headspace volume before headspace oxygen.
- Squeeze the headspace air gently into the form of a cone
64
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Measuring headspace volume
Position the BIB Cone Meter and measure the two sides of the cone (in cm)
Calculate the average in cm and read the corresponding volume of the cone in mL from the
BIB Cone Meter.
ml
cm
44.1
50 0
50.0
56.4
63.3
70.6
78.6
5.50
5 75
5.75
6.00
6.25
6.50
6.75
87 0
87.0
7 00
7.00
Abracadabra!
65
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Measuring headspace volume
For the special case of metallized bags,
remove the outer metallised film layer with the help of a cutter and a pair of scissors –
preferably without piercing the bag!
66
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Measuring headspace volume
For the special cases of bags:
- with rounded corners (welds), measure the full cone to the apex and then deduct the
volume of the missing corner (generally < 2 mL)
- filled with a lot of foam, preferably wait for the average foam thickness to settle under
5 mm and then measure from the bottom of the foam. Alternatively subtract from the
total headspace (measured from the bottom of the foam) the liquid equivalent of the
f
foam.
This
Thi liquid
li id equivalent
i l t iis calculated
l l t db
by estimating
ti ti th
the volume
l
off th
the ffoam ((using
i th
the
cone meter) and multiplying the foam volume by a coefficient (we use 15%).
67
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
A simple rule of thumb using the BIB cone
meter
Bag‐in‐Box ®
Cone meter
Cone meter
Green Zone:
U tto 5 cm
Up
Excellent!
Yellow Zone:
> 5 cm tto 7 cm
OK but improve!!
Red zone:
> 7 cm D
Danger!!!
!!!
(unless your % of oxygen is very low)
68
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Measuring headspace oxygen with electrodes
- Place some tape on the aircone in the spot where it is to be pierced.
- Pull an air sample slowly into a syringe and inject immediately (but slowly) into
measurement chamber for % O2 reading.
- there is an underlying hypothesis that the internal pressure of the BIB aircone is similar
to the pressure inside the measurement chambre but this is probably the case for BIB
BIB.
69
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Measuring headspace oxygen with an optode
Using optical instruments:
- Carry the BIB gently from the filling machine to a measurement table located as close as
possible to the filling machine
- For the measurement, secure the BIB (with the tap above) with the help of a holding
p
clamp
- Make the measurements immediately after filling
70
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Measuring headspace oxygen with an optode
Using optical instruments:
- We consider the values to be acceptably stabilized within 2 minutes for most
situations
- Record the oxygen result in %. The simplicity of using a value in % could be a source
pressure inside the p
package
g was very
y different than the total p
pressure
of error if the total p
used for the calculations (by the optode) but this is generally not the case with BIB
packaging.
71
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Calculate headspace oxygen in mg/L
After having measured the % of oxygen in the cone using an oxygen sensor (= % O2):
Calculate the quantity of oxygen in the cone (mg/L) using the following formula:
(% O2) x (volume headspace mL ) x (1.429 mg O2/mL O2)
-------------------------------------------------------------------------volume BIB (L wine)
The result is an expression of the reserve of O2 in the cone that could potentially be
transferred to the wine.
72
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Calculate DO with electrodes
Using electrochemical instruments:
- Put the BIB in a box with the tap below
below, at a
height of about 1 meter above the O2 meter.
- The debit of the wine exiting the O2 meter should
be regular and sufficient (10 L/h)
L/h). If not add a
peristaltic pump after O2 meter.
- Wait until the circuit is purged of any air
- When the measures are stable
stable, record them in
ppm (mg/L)
73
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Calculate DO with optodes
Using optical instruments:
- Hold the BIB with the tap below
below, with the help of a holding clamp in such a way so that
only wine (and no air) is filling the tap.
- Make the measurements as soon as possible after the headspace measurements.
74
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Stabilisation time for DO readings with optodes
This stabilisation period for DO (between the beginning of the masurements and when
they refect reality) must still be further studied
studied.
Some sources recommend between 0 and 40 minutes.
This delay must be long enough so as to eliminate the effects of any micro-air bubbles on or
around the sensor spot, but the delay must not be so long as to introduce other errors
including too much consumption of the oxygen by the wine. In addition, wineries practices
generally impose no longer a wait than truly necessary.
At this stage of our research, we recommend a stabilisation time of 15 minutes for DO
readings
di
((non agitated
i
d wine)
i )b
but this
hi recommendation
d i may change
h
as ffurther
h tests are
conducted.
75
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Stabilisation time for DO readings with optodes
Typical DO in unshaked BIBs drops rapidly the first 5 minutes in non-skaken BIB wine and
then DO drops more slowly as time goes on
on. As indicated
indicated, our recommended stabilisation
time (waiting period) is15 minutes before accepting that the DO value is valid.
76
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Stabilisation time for Headspace readings with optodes
Typical headspace readings appear to be very stable immediately. The graph below is for
the same wine BIB as the previous slide (shown for DO)
77
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Stabilisation time for agitated wine with optodes
After agitation (on an orbital shake table at 275 RPM for 4 minutes), TPO (DO +
Headspace) values are very stable immediately
immediately. Readings of initial headspace oxygen
before agitation should also be taken.
78
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Recommended stabilisation times
The table below summarizes our recommendations:
Type of
mesurement
Electrochemical
Technologies
(electrodes)
Optical technologies (optodes)
With t agitation
Without
it ti
With agitation*
it ti *
Dissolved O2
Immediate
15 minutes
Immediate
Headspace O2
Immediate
2 minutes
Immediate
* Agitation
g
with orbital shaker table at 275 RPM for 4 minutes.
79
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Timing and steps for O2 measurements with optodes
Times provided below assumes that the instrument is already calibrated, sensor spots are
already glued,
glued recommended stabilisation times are applied and the tester is experienced
experienced.
The initial DO test (if only one measurement is taken) will take at least 25 minutes and TPO
((headspace
p
oxygen
yg and DO)) in filled BIBs will take a minimum of another 30 minutes p
per BIB.
1st step: Measure initial main wine tank DO (stabilisation time 15 minutes + set-up and
recording time approx. 10 minutes)
2nd step: Measure headspace oxygen immediately after filling (stabilisation time 2 minutes +
set-up and recording time approx. 3 minutes)
3rd step: Measure headspace volume (set up and measurement time: approx. 5 minutes)
4th step: Measure of filled package DO level (stablisation time: 15 minutes + set-up and
recording time approx. 5 minutes)
If an orbital
bit l shaker
h k is
i used,
d overallll measurementt titime iis shortened
h t
db
butt results
lt th
thus obtained
bt i d
may have to be intrepreted differently than results from tests without skaking.
80
Wine BIB O2 measurements /Part 3: Recommended Procedures /3.3 Headspace O2 and DO
Some TPO Profiles
A comparison of Total Package Oxygen (TPO) in wine BIBs right after filling, observed
at various wineries
mg/L O2
16
14
12
10
8
6
4
2
0
Headspace Oxygen
DO pick‐up
Initial DO
1 2 3 4 5 6 7 8
High Excellence
Not OK
8 different profiles
81
Wine BIB O2 measurements / Part 4: Future Research
Part 4: Future research, by Patrick Shea, Vitop
82
Wine BIB O2 measurements / Part 4: Future Research
Can we accurately predict wine BIB shelf life?
 Not yet
BIB Shelf life correlation has been established:
 Reasonably well for: - SO2 levels
- Microbiological growth
- DO pickup during filling
- Temperature
 Somewhat for:
- The type of wine
- Package damage
 Very little for:
- Air cone oxygen
- Package OTR
Shelf-life predictions do not appear to work very well when based upon gas/gas O2
transmission rates of the barrier film and tap and we know little about the real impact of
varying levels of air cone oxygen (volume or % O2).
83
Wine BIB O2 measurements / Part 4: Future Research
The BIB industry needs to improve its O2 metrics!
“Dry Test (gas/gas)” OTR results do not reflect real conditions for liquid packaging and often
do not appear to be very good indicators of expected shelf-life
shelf-life.
Although some studies do show an overall correlation between “Dry Test
(gas/gas)” OTR results and shelf life, we also have:
- The extensive 2004 INRA testing for Performance BIB where a special
sealing wax placed over the tap reduced gas/gas OTR by about 42%
relative to the unsealed taps. No impact on wine shelf life was observed.
- Several shelf life tests with various films having very different “Dry Test
(gas/gas)” OTR results but with little impact on wine BIB shelf life.
Left: comparison
p
between two
types of BIB bags (inserted or not
in boxes) having different “Dry
Test (gas/gas)” OTR results with
no difference in shelf life.
Presented by C
C. Schussler
(Geisenheim Wine Research
Centre) at Performance BIB
general meeting in 2008. 84
Wine BIB O2 measurements / Part 4: Future Research
Need for future research
Create model solution (for example, low oxygen, high acid water) in BIB package.
Vary key parameters (headspace oxygen % and
volume, DO, CO2 levels, film barrier properties, etc.) in
both the model solution and BIBs filled with wine to
establish clear correlations between changes
g in DO
levels in the model solution and changes in the wine.
The wine would be evaluated both analytically and
sensorial,, using
g also the same wine in a glass
g
bottles as a benchmark. This can build upon the filled
package research already pioneered by Georges
Crochiere, Aurélie Peychès Bach, Jean-Claude Vidal
and others.
mg
g/L or ppm
m O2
Conduct parallel tests with wine to determine the true correlation between Total Life Cycle Package
Oxygen (see schema page 22) in the model solution (in mg/L) and wine BIB shelf-life (and also
establishing the degree of correlation with Dry Test OTR results).
3,50
3,00
2,50
2,00
1,50
BIB Bag 1
BIB Bag 2
1,00
,
0,50
0,00
0
10
20
30
40
50
days
85
Wine BIB O2 measurements / Part 4: Future Research
Need for future research
Through better oxygen measurement systems, we can pinpoint further
areas of improvement and extend wine BIB shelf-life
O2
O2
Shelf life goal:
Bell curves tightened (less variance)
and/or shifted to the right
N° of BIBs
N° of BIBs
Total Life Cycle Package Oxygen goal:
Bell curves tightened (less variance)
and/or shifted to the left
O2
O2
mg/L
A
Shelf-life (in months)
86
Wine BIB O2 measurements / End
For more information contact:
Patrick SHEA
vitop 
Tel +33 4 67 59 82 18
Tel.
ps@vitop.fr
Sophie VIALIS
Tel. +33 4 90 11 46 00
svialis@inter-rhone.com
Jean-Claude VIDAL
Tel. +33 4 68 49 44 00
vidaljc@supagro.inra.fr
Photo:
Office de Tourisme de Bordeaux
T. Sanson
87