HEINEKEN VIETNAM BREWERY LTD

TEC.SD.51.12.01 Page: 1 - 8

TEST METHODS & REQUIREMENTS FOR LABEL GLUE

The chapter covers some basic and specific test methods and requirements, which are applied for inspecting and testing
the label glue at HVB and the supplier to ensure the conformity of its quality.

1. Odor
This may not have any harmful effect on the people who handles the labeler and on the product to be glued.
Inspection instruction: Open a glue drum to smell its odor.
Requirement: no strong harmful odor (for health), slight ammonia compound is acceptable.

2. Color
This may not effect the passage of light through the label after drying.
Requirement: white milk color.

3. pH
The neutral medium is required in order to prevent any corrosion for the machine. pH is checked by pH meter.
Requirement: pH = 7.5 – 8.5

4. Penetration (HMESC 06.94.02.002)

The adhesive is visible through the label
Requirement: not visible
Inspection instruction:
4.1 Store bottles labeled with the adhesive under normal store conditions for 2 days.
4.2 Spread the CuSO4 solution (blue color) over the surface of label.
4.3 The adhesive will be colored blue by CuSO4 solution. This makes visual observation of penetration easier.

5. Viscosity (static)
The test is to measure the viscosity of glue at normal working condition.
Requirement: 85,000 – 150,000 cps at 27C.
Inspection instruction: 500 ml of glue is taken in the beaker of 500 ml. The viscosity is measured by
viscometer Brookfield RV, spindle 7 at 27C, 20rpm. After the desired temperature has been observed, use
chopsticks to stir slight 3-5 rounds in order to remove the surface of sample and then measure viscosity.

6. Viscosity (dynamic)
Under pumping condition, the glue property may be changed due to the shear force. In other word, the glue
viscosity may be reduced but not significant.
Requirement: 50,000 – 100,000 cPs at 27C
Inspection instruction: Measure viscosity after 1-hour continuous pumping at 25 - 30C by viscometer (see
point 5)

7. Dissolubility in caustic solution 3% w/v at 80C

The test is to check the dissolving ability of wet glue in washer and whether the glue causes precipitation or
gelation in the hot caustic solution.
Requirement: <= 60 seconds for complete dissolve and clear solution.
Inspection instruction:
7.1 Heat up 100 ml of 3% caustic solution to 80C.
7.2 Place about 5 g of glue into the caustic solution, start the stopwatch and stir the solution regularly.
7.3 Stop the stopwatch if the glue is completely dissolved in the solution.
7.4 Note the time and observe the clearness of caustic solution.

8. Setting Time (HMESC 06.94.02.002)

This is the ability of adhesive to hold the label on the bottle at the start of fiber retention occurs.
Requirement: <60 seconds
Inspection instruction:
8.1 Take the bottle just after labeling and start the stopwatch at the same time.
8.2 Stop the stopwatch if the fiber retention occurs when peeling off the label.

9. Drying Time (HMESC 06.94.02.002)

The time that elapsed between the application of label on the bottle and the time when the label is removed at
least 50% of the fibers from the paper surface remaining on the glass is called drying time.
Requirement: < 6 minutes

Doc No.: TEC.SD.51.12.01

Author: DCNguyen_TE
Issue: 4
Approver: NTHUYEN_TCPM
Eff. Date: 31-May-2018
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TEC.SD.51.12.01 Page: 2 - 8

Inspection instruction:
9.1 Take the bottle just after labeling and at the same time, the stopwatch is started.
9.2 Pull the label from the left to right to remove it from the bottle after every minute.
9.3 Visually assess the extent at 50 % of fiber retention.

10. Glue tackiness (Cohesion) (Quick method)

It is a hand feeling peeling off force. The glue tackiness should be as high as possible to maintain the position
of label just after labeling under pressure of brushes and movement. However, it should not be too strong to
labeling, resulting dropped label at labeler, glue splashing, etc.
Inspection instruction: Peel off the label to assess the cohesion of glue.

11. Solid content

The amount of dry matter is in 100 g of wet glue.
Requirement: 35 – 45 %
Inspection instruction: The solid content is measured by dryer Mettler PM 300.

12. Consumption
The wet glue quantity is essential for labeling.
Requirement: 15 – 25 g/m2 label.
Inspection instruction:
12.1 Stop the glue pump in labeler.
12.2 Note the quantity of running bottle in labeler (B1, bottle).
12.3 Weight the glue drum by digital balance with two decimal numbers (W1, gram).
12.4 Switch on the glue pump and let the labeler run for at least 2 hours.
12.5 Stop the glue pump, note the quantity of running bottles, and drum weight again (B2 & W2).
12.6 The consumption of glue is calculated as follows:

(Other method is to keep the pump run during reading, depending on condition of labeling, any method can be
used).

100 x (W1 – W2)

Consumption (g/m2) =
A x (B1 – B2)
in which:
A (dm2): total label area that those labels are glued by the weighted glue drum.

Area, dm2
Type HP TP T50 TQ Biv
Body 0.613 0.572 0.697 0.786 0.902
Back 0.471 0.375 0.375 0.375 N/A
Neck/Foil 0.134 0.120 N/A N/A 0.165
Foil N/A 0.540 0.640 0.840 N/A

13. Cleanability (HMESC 06.04.02.002)

The adhesive must, in either the liquid or the dried condition, be readily soluble in water at 40C and easily
removed using a brush.

14. Labeling performance (HMESC 06.09.02.002)

The glue should not be splashed or flagged during process. The label should have a flat surface after gluing
(no wrinkle).

15. Ice-Water resistance (7 days – Heineken method - HMESC 06.94.02.002)

This is a standard test to evaluate the label adhesion to the bottle.
Requirement: <= 15% dropped label after 7 days in cold water (0 - 5C)
Inspection:
15.1 Take randomly 40 labeled bottles at the normal speed of labeler during production.
15.2 After a drying period of 07 days at the room temperature, place the labeled bottles in the cold water bath 0 -
5C (tap water) in such way that the labels are at least 10 mm under the water level. The distance among the
bottles should be a minimum of 20 mm. The bottles stay motionless in the water bath.
15.3 Every day rotate, the bottles gently haft turns to and fro without the bottle knocking against each other.
The bottles must remain under water during this operation.

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15.4 Record and sum up the number of dropped label in the bottle every day.
15.5 Express the result as a percentage of total loose labels of total labels to be tested.

16. Ice-Water resistance (21 days – HVB method)

This is a standard test to evaluate the label adhesion to the bottle.
Requirement: <= 15% dropped label after 21 days in cold water (0 - 5C)
Testing requirements:
 Drying period: 04 days at room temperature.
 Water: cold water 0 - 5C (tap water) or cool water bath with stable water flow.
 Glue thickness: 80 – 100 µm.
Inspection:
16.1 Take randomly 20 labeled bottles at the normal speed of labeler during production.
16.2 After a drying period of 04 days at the room temperature, place the labeled bottles in the cold water bath 0 -
5C (tap water) in such way that the labels are at least 10 mm under the water level. The distance among the
bottles should be a minimum of 20 mm. The bottles stay motionless in the water bath.
16.3 Every day rotate the bottles gently haft turns to and fro without the bottle knocking against each other. The
bottles must remain under water during this operation
Record:
 Record and sum up the number of dropped label in the bottle everyday. Express the result as a
percentage of total loose labels of total labels to be tested.
 Record glue thickness, glue information (Prod. Date, batch...) and water temperature

17. Ice-Water Resistance with Crushed Ice (HMESC 02.13.02.032)

This method describes a standardized test for the evaluation of Ice-water Resistance of labels using crushed
ice and melt water that is formed. This is more consistent with consumer habits in order to cool the beer: the
bottles are put into crushed ice for sometime. It was found that mechanical forces due to the crushed ice are of
great influence on the ice –water resistance of labels.
Requirement: <= 15% dropped labels after 4 days
Inspection instruction:
17.1 Preferably start the test on Friday; if this is not possible, the test can start any other day.
17.2 Take randomly 12 labeled Heineken bottles at the normal speed of labeler during production.
17.3 Mark the bottles on the crown from 1 – 12 with a water-resistance marker.
17.4 After drying period of 4 days at the room temperature, place the labeled bottles in the cool box in such way
that the bottles do not affect each other during the test.
17.5 Fill the box with an excess of crushed ice and place the cover. All labels must be completely immerged in ice.
17.6 Place cool box in a cold storage at about 4C. If a cold storage of 4C is not available, the box should be place
in a cool place but not less than 4C.
17.7 Drain excess of the melt water and fill up the crushed ice every 1 to 3 days depending on the outside
temperature. The labels on the bottles must always be surrounded with crushed ice AND melt water.
17.8 Rotate the bottles everyday on the following day:
One full turn right and one full turn left, followed by one full turn right.
After this, pull the bottle out of the ice and roughly estimate the percentage label area that came loose of the
label to be tested.
17.9 Push back the bottle into the ice, turn the bottle one full turn left and repeat the rough estimation of the
percentage of loose label area.
17.10 To record the data use the table given in appendix 1.
17.11 The duration of the test is 2 weeks, unless all labels have already come off before the end of the test period.
17.12 For each label type (body, back and neck), sum up the percentages for the individual labels of bottle 1 up to
and including bottle 12 and express this sum as a total percentage of the surface of the 12 labels to be tested
(i.e. total percentage of the surface of the 12 labels to be tested = 12 x 100% = 1,200%).
17.13 The number of labels that came off the bottle is summed and is expressed this sum as a percentage of total
labels to be tested.
17.14 Compare the results of this method with tests done under local conditions.

18. Salt-Ice-Water Resistance (HVB method):

The test is used to evaluate label adhesion to the bottle in the salt solution 2% g/L, which is the practical
method to cool the beer in the market.
Requirement:
 No label dropped in first 8 hours.
 >3 days at 100% label dropped.
If salt IWR test failed, conduct the standard method of 21 days to work further with Supplier.

Doc No.: TEC.SD.51.12.01

Author: DCNguyen_TE
Issue: 4
Approver: NTHUYEN_TCPM
Eff. Date: 31-May-2018
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TEC.SD.51.12.01 Page: 4 - 8

Inspection:
18.1 Take randomly 40 labeled bottles at the normal speed of labeler during production.
18.2 After a drying period of 04 days at the room temperature, place the labeled bottles in the cold water bath 0 -
5C (tap water) in such way that the labels are at least 10 mm under the water level. The distance among the
bottles should be a minimum of 20 mm. The bottles stay motionless in the water bath.
18.3 Every day rotate, the bottles gently halt turns back and forth without the bottle knocking against each other.
18.4 The bottles must remain under water during this operation.
18.5 Record and sum up the number of dropped label in the bottle every day.
18.6 Express the result as a percentage of total loose labels of total labels to be tested.
Calculation result
% drop label = (total dropped labels/total labels tested) *100

19. Rolling Ball Tack Test (HVB method):

In this procedure, a rolling object (a steel ball according to this standard, but other geometries and materials
are also possible) is placed at the top of an inclined track pursued by a horizontal, upward-facing adhesive.
The ball is rolling down, and the relevant measurement is the distance the ball travels along the adhesive tape.
This simple, but frequently used, test is probably one of the oldest. Despite its simplicity, it gives a good idea
of the adhesive behaviour and is readily understood. This distance is inversely proportional to tackiness: the
greater the distance, the less tacky the adhesive.
But this test can only be applied as an internal comparative test, because there is no information about
adhesive surface or bulk parameters. And different attempts to summarize bibliographic data (using balls of
different sizes, composition, texture,...) have not given (for instance) a good mechanical model, reliable
measurement and adhesive properties.
Practically, the measurement needs to be performed several times to obtain average values and a significant
result. For many adhesives, a wide range of results are obtained; moreover, often the maximum prescribed
distance in the standard is lower than the experimental one. The method by itself is low cost and easy to use,
but often needs to be adapted to the parameters of the real system (temperature, tack capacity,...). It is also a
good quality control for tapes, for example.

Loop Tack Test

In this test, tape samples are circular loops and caught in the upper jaw of a tensile tester. This pear or teardrop
is brought into contact with a horizontal surface (model or real system) for a short conventional time, and then
peeled off.
As for the rolling ball test, variations near this scheme are possible: shape of the substrate, pressure applied,
for example. The main advantages of this test are that it is easily and quickly performed, does not require
specific equipment (a standard tensile tester is sufficient), and the reproducibility is in most cases acceptable.
When equipped with an environmental chamber, one can also vary contact conditions, and in this way, study
their influence.
But drawbacks are originated from the method itself: contact time and peel angle are difficult to reproduce,
and the stiffness of the tape backing is also strongly influent.

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Author: DCNguyen_TE
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Approver: NTHUYEN_TCPM
Eff. Date: 31-May-2018
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In summary, the loop tack test is a good means of measuring the tack of labels or tapes when the applications
are confined to the experimental conditions.
Advantages Drawbacks Applications
Influence of
Medium cost
backing
(requires a
Care must be Choice of the adhesive,
dynamometer)
taken to especially for labels or
Good precision and
reproduce closed applications
reproducibility
pressure and area
Easy to explain
of contact
Loop Tack Test

Peel tack test

Derived from the standard peel test (but time and pressure of contact are lower), it can be compared with the
previous test (but in this case, the operator itself puts the adhesive on the adherend surface).
The equipment required is the same as that for the loop tack test, except that a reproducible pressure must be
applied. If it is slightly less quick to carry out, a better reproducibility is achieved because of a better control
of contact conditions and of peel angles. It really becomes possible to compare peel measurements at different
contact times and pressure, and to extrapolate at zero time of contact to obtain an "absolute" value.

Nevertheless, the stiffness of the backing is also influent, and the results depend not only on adhesive
tackiness, but also on the tape modulus. To summarize, peel tack test can be interesting, but one can be far
from a real tack test if pressure and time of contact are too high; as with other tests, one must be as near as
possible to the usual conditions.
Advantages Drawbacks Applications
Medium cost
(requires a Influence of
Choice of the adhesive,
dynamometer) backing
especially for labels or
Good precision and Difficult to study
closed applications
reproducibility low contact time
Easy to explain
Peel Tack Test

Probe Tack Test

The simplest equipment to evaluate tack properties is a thumb. Brought into contact with a slight pressure and,
after a short delay, pulled away from the adhesive, the sensation of tackiness felt by the operator can be
reported on a scale of, by example, 0 (no tack) to 5 (very aggressive tack). But it is obvious that this method is
not reproducible: each operator has his own appreciation, varying according to the day or his own senses.

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So, although more precise sensors and more reproducible probes are preferred, the idea is the same.
Mechanical probe tack testers bring a probe (ball or cylinder of various material) into contact at controlled rate
and pressure, wait a given delay, and measure the force needed to pull away at a specified rate. Most systems
allow each individual parameter involved in the bond formation to vary (the ASTM D2979-00 is related to the
first experimental equipment, called "Polyken Probe Tack").

One can obtain this figure, reporting the measured force during the experiment.

It is very interesting to understand the phenomena observed during the separation between a tacky adhesive
and an adherend.
a) the stress increases linearly with the probe displacement,
b) the stress slowly increases and is no longer linear, because a nucleation phenomenon occurs (apparition of

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voids at the interface),

c) the force goes up to a maximum, when the nucleation stops,
d) cavities start to grow perpendicular to the interface, involving a decrease of the stress; at this stage, the
shape of the curve depends on the rheological properties of the adhesive and on interfacial interactions
between the adhesive and the probe; there are two possible ways for debonding to occur:
e) voids can grow until coalescence occurs: in this case the failure is adhesive and the stress decreases to zero,
f) or cavities can grow to reach a critical size, and fibrillation appears. Fibrils can lead to adhesive failure (f2)
or cohesive failure (f1)
In this method, the experimental parameters are the same as during a real bonding process :
contact pressure;
contact time;
temperature;
rate of separation;
probe used (shape, material,...);
and obviously the adhesive system (thickness, backing, roughness,...)
Although the results are more difficult to analyse, this method is a precious one: the use of a dynamometer
gives high precision and the parameters (forces at different contact times, but also energies of debonding) can
lead to a better understanding of the PSA behavior.

Advantages Drawbacks Applications

High cost
Very versatile
Specific
Good sensibility and
Careful preparation applications
reproducibility
of samples Formulation,
A lot of information is
Needs time to be compounding
accessible
performed Research
Possibility of varying each
laboratory
experimental parameter
individually
Probe Tack Test

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Author: DCNguyen_TE
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Approver: NTHUYEN_TCPM
Eff. Date: 31-May-2018
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TEC.SD.51.12.01 Page: 8 - 8
Appendix 1: Example table with data recorded during the first three days of the 14 days test period.

Sample : Amstel Light (bottle date: 15/11/2002)

Start date : 19/11/2002
Glue : Body + Back: NS-cycloflex 14-201A
Neck: NS495/110/01
Glue thickness : Body 100µm; Neck 100µm; Back 80µm
Water temperature: 4oC

Bottle Day 1 Day 2 Day 3

% label off Completely off % label off Completely off % label off Completely off
Body Back Neck Body Back Neck Body Back Neck Body Back Neck Body Back Neck Body Back Neck
1 0 5 20 0 0 0 0 20 20 0 0 0 10 25 20 0 0 0
2 0 0 100 0 0 1 10 10 100 0 0 1 20 20 100 0 0 1
3 0 5 25 0 0 0 0 10 25 0 0 0 0 10 25 0 0 0
4 0 0 25 0 0 0 0 5 25 0 0 0 0 20 100 0 0 1
5 0 10 25 0 0 0 10 100 25 0 1 0 10 100 30 0 1 0
6 0 0 20 0 0 0 5 10 100 0 0 1 10 10 100 0 0 1
7 0 5 10 0 0 0 5 10 10 0 0 0 10 20 10 0 0 0
8 0 5 10 0 0 0 0 20 10 0 0 0 10 20 10 0 0 0
9 0 5 100 0 0 1 25 20 100 0 0 1 100 30 100 1 0 1
10 0 5 25 0 0 0 10 25 25 0 0 0 10 100 25 0 1 0
11 0 5 20 0 0 0 10 10 20 0 0 0 10 25 20 0 0 0
12 0 5 10 0 0 0 10 10 10 0 0 0 20 25 20 0 0 0
SUM 0 50 390 0 0 2 85 250 470 0 1 3 210 405 560 1 2 4
Total % 0 4 33 7 21 39 18 34 47

Doc No.: TEC.SD.51.12.01

Author: DCNguyen_TE
Issue: 4
Approver: NTHUYEN_TCPM
Eff. Date: 31-May-2018