FTM25

evaluation of the silicone

coverage of coated papers by use
of a water based stain test

scope test equipment

This test method describes a technique for assessing the Cobb Tester with ring of an approximate diameter of
quality of coverage of silicone coatings. This test can only 11.5cm.
be carried out on paper based liners which can be coloured
by the stain test solution utilised. Count down stopwatch with alarm function.

Small container, marked to show level occupied by 200ml

definition of Stain.

Silicone coverage quality is commonly evaluated by water Test stain solution.

soluble dye stain testing.
There are many dye stains used, available both in solution Absorbent cleaning paper.
(which can be directly used), and powder form (which
must be prepared). These include Shirlastain ‘A’, Malachite
Green, Methylene Blue, Hahn Stain, Rhodamine 6 GDN and test pieces
Neocarmine A).
Where possible, several samples should be evaluated from
For paper substrates only, a quantity of liquid dye stain is the release sheet.
applied to the silicone coated liner for a finite period of If these are from a known position on the web their
time, rinsed or wiped off and the liner dried. location should be noted for reference.
Coverage is then determined by visual inspection or by
colorimeter (for a more quantitative measurement). In
general the darker the coloration from the stain solution, test condition
the poorer the silicone coverage.
No special conditions apply.

procedure

   

Stain solution Preparation

If a pre-prepared stain solution is used (such as “Shirlastain

FINAT TECHNICAL HANDBOOK 2014 |

A”), then no stain solution preparation is necessary and the

solution can be directly used.
For all other dyes a stain solution needs first to be
prepared. The following steps outline the procedure to
prepare a ‘typical’ stain solution where the concentration
level of dye is approximately 0.5 wt%;

52
a. Take a 1litre container (a capped polyethylene bottle is
suitable), and place on an electronic balance.
b. Wearing the appropriate safety equipment*, and
taking care when handling the dye, weigh out carefully
5g of dye into the container (Malachite Green Oxalate,
Neocarmine A, Methylene Blue or Chrystalline Violet
are some of the recommended materials).
c. Measure out 1 litre of distilled water using the
measuring cylinder and add to the container. Seal and
shake the container thoroughly to dissolve the dye.
*Safety comment – Particular care should be taken to read
and follow the safe handling instructions for the dye as
many of the materials are hazardous in their pure state.
Although the final 0.5 wt% dye solutions are not usually
considered hazardous, it is still recommended to wear
protective gloves when handling them.
Coverage test
1. Cut a 14 cm x 14 cm (or size suited to Cobb tester
used), sample of release liner (or liner of self-adhesive
laminate after removal of face material). Care must be
taken to ensure that there are no holes or perforations
present in the backing paper. In all cases, regardless of
the substrate or dye being used, care should be taken
to avoid contact with the silicone surface prior to
testing since this may introduce imperfections in the
stain result.
2. Place the release liner sample on the base of the Cobb
tester, silicone side up, under the test ring.
3. Clamp the rind securely in place to prevent the stain
leaking out during the test.
4. Add 200ml of the ‘Stain’ solution into the Cobb tester
and start the stopwatch / clock. The ‘exposure’ time
used should be adjusted to suit the dye solution
but also the type of substrate paper and silicone
coat weight, but see below for some typical starting
recommendations for the different stains.
Neocarmine A – an exposure time of 60 sec is typical.
Methylene Blue – an exposure time of 120 sec is
typical
Malachite Green – an exposure time of 60 sec is
typical
Shirlastain ‘A’ – an exposure time of 120 sec is typical
5. At the end of the specified ‘exposure time’ chosen
for the test, immediately drain off the stain solution,
unclamp the test ring and lift it away from the sample.
6. Blot the test piece dry with absorbent paper or cotton
swab (DO NOT RUB), and allow the dried sample
to sit for a further five minutes (method usually
recommended with Shirlastain ‘A’), before examining
or making measurements on the sample.
Alternatively the sample can be rinsed under a
running tap and then blotted dry (method usually
recommended with Malachite Green). Once dry the
sample can then be examined / measured.
results
The visual assessment of the sample should be to assess
for general level of colour of the sample and to look for
evidence of dye penetration into the base paper. For
good silicone coverage there should ideally be NO sign of
penetration by the stain solution. Penetration of the stain
is identified by the appearance of dark lines or spots. The
deeper and more visible the stain, the greater the risk of
an adhesive being able to penetrate through the release
coating and into the base substrate, which will could
cause issues with release force (leading possibly to label
dispensing failures, tape release problems etc.).
If the particular sample being tested is deemed satisfactory
in all other performance requirements, then it should
be used as a benchmark for future tested samples. Each
backing paper type should have it’s own benchmark
sample for comparison (i.e. a silicone coated liner where
the performance is deemed acceptable and where the
stain test has been carried out). Future tests can then be
compared against the benchmark sample (or range of
samples if a more precise rating is required), and results
should be the same as or better than the ‘acceptable’
coverage benchmark. It is also possible to use this test to
establish a graded ‘scale’ of silicone coverage from 0 – 10
where;
• ‘0’ = Total stain of paper surface equivalent to that of
unsiliconised paper
• ‘10’ = Perfect stain with no sign of coloration
FINAT TECHNICAL HANDBOOK 2014 |
(Yellow glassine paper with different levels of silicone coverage,
stained with a solution of Methylene Blue.)
53
 FTM25
evaluation of the silicone
coverage of coated papers by use
of a water based stain test

The ‘acceptable’ level of coverage would need to be set

depending on other product performance criteria.

For a more quantitative measure of silicone coverage, the

degree of coloration of the coated paper sample may be
used. A colorimeter should be used to measure the colour
‘vector’ values for the sample and then compared against
the same measurement for the uncoated base paper to
give a “Delta – E” value for the sample. A specification may
then be set on the target “Delta – E” that is acceptable.
Though this method can give a quantification of the stain
test, attention must still be paid to the regularity of the
coverage (to look for defects in the coating), as the colour
measurement only gives an ‘average’ of the surface. The
usual approach is to accompany the colour measurement
on the sample with a descriptive comment about the
sample.

safety
It is strongly recommended to carefully read and follow
the Safe Handling instructions for the dye being used
(especially when handling the undiluted dye during
solution preparation). In addition, it is recommended to
always wear protective gloves , even when handling the
final dye solution.

notes
The most commonly used dye solution is Malachite
solution. This based on using the dye Malachite Green
Oxalate (Basic Green 4), C.I. number 42000. Malachite
solutions should be stored in well closed containers and
kept away from exposure to daylight. Storage life of the
solution is about 1 month.
Alternative dyes could be used to replace Malachite Green
Oxalate, such as;
• Chrystalline Violet
• Methylene Blue
• Neocarmine A – Recommended for yellow coloured
liners as the colouration is red
If a pre-prepared dye solution is preferred, then one
recommendation is to consider SHIRLASTAIN ‘A’ which is
FINAT TECHNICAL HANDBOOK 2014 |

supplied by.

SDL Atlas Ltd.

www.sdlatlas.com.
For addresses please consult section 3.3. of this book.

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