En-12004 Impac On Adhesive Formulations
En-12004 Impac On Adhesive Formulations
En-12004 Impac On Adhesive Formulations
GREATER DEMANDS
The impact of the new EN 12004 standard on formulation
technology and raw materials for cement-based tile adhesives
Contents
Background
Summarised results
Cement
Sand
Cellulose ethers
Experimental
Test methods
New Standards Make Greater Demands
The aim of the study is to provide The results of studies relating to experience, because of insufficient
you with data and guidelines to EN 12004 depend not only on the adhesion after heat aging.The
assist you when carrying out tests adhesive being tested, but also quantity of polymer powder can
on cement-based tile adhesives in strongly on the type of tiles and be reduced when cement of higher
relation to compliance with EN concrete slabs used.This fact must quality is used (Table 1).
12004. be taken into consideration with
regard to the «absoluteness» of the It is far more difficult to formulate
The following table (Page 2) provi- test results. Obviously the materials tile adhesives meeting the C2
des an overview of the require- used for the tests should meet classification. Tensile adhesion requi-
ments per classification of cement- the specifications required by the rements of >1.0 N/mm2 represent
based tile adhesives. norms. quite a challenge. The results of our
The general classifications C1 and studies allow the following conclu-
C2 can be combined with additional It is relatively simple to formulate an sions to be drawn:
requirements (F,T, E). adhesive which meets the C1 requi-
2 Designations like C1T or C2TE rement. It is not a great obstacle to • The tensile adhesion strength can
clearly describe the properties of reach the required 0.5 N/mm2, but be improved by the use of higher
cement-based tile adhesives. Rapid the challenge is rather that of kee- quality cements. An important fact
hardening adhesives (F) were not a ping the cost as low as possible. to be taken into consideration is
subject of this study.The freeze-thaw Aiming to omit the polymer powder that the increase in tensile adhe-
cycle was also omitted, as manually from the formulation would be sion, after water immersion or
executed freeze–thaw yields results attractive from an economical point after heat aging, increases dispro-
with limited reproducibility. of view but would fail, in our portionately.
Note: Please refer to the original Std. EN 12004 as reference.This is just an interpretation by Dow.
Making Sense of Euronorm
EN 12004 – A Synopsis
Portland cement is available in many Portland cement quality from CEM I proven that the tensile adhesion,
quality classifications. Depending on 42.5 to CEM I 52.5, the standard after these two aging procedures,
the particle size and the chemical tensile adhesion improved only are the most critical properties
composition of the clinker, concrete slightly, by an average of 0.2 N/mm2. in order to meet EN 12004
with different compressive strength Comparing the tensile adhesion requirements. Surprisingly the
values is obtained. Fine particles results in the same set of tests, nominal improvement of the tensile
will hydrate better, thus yielding after 20 minutes and 30 minutes adhesion is independent of the
5 higher strength values.This effect open time, no difference can be redispersible polymer powder level,
can also be observed in cement- determined. which means that the increase in
based tile adhesives as the following tensile adhesion strength which is
table demonstrates: Results obtained after the water influenced by the cement quality,
immersion test (+0.3 N/mm2) and is the same for both the formu-
Results: The influence of the after heat aging (+0.5 N/mm2) lations containing 1% DLP 2000 and
Portland cement quality on the demonstrate that the use of 3% DLP 2000.
tensile adhesion results is not so better quality Portland cement
evident in all tests. Changing the can be advantageous. Practice has
Properties
Slip mm 2.0 2.0 4.0 3.0
Tensile adhesion strength
Standard N/mm2 0.88 1.05 1.39 1.56
20 min open time N/mm 2
0.86 1.02 1.39 1.34
Water immersion N/mm2 0.70 1.02 0.69 1.01
Heat aging N/mm 2
0.15 0.65 1.00 1.50
Table 1: Comparison of two different cement qualities with two different DLP 2000 levels
Because of the relatively high mm) and a substantially higher Ground limestone (~60 µm) is often
transport costs, the choice of sand specific surface (~ 2.9 m2/g). added to the formulation as a fine
remains limited to local sand filler to improve the application
supplies. Nevertheless, it makes Results: Comparing the two properties and a better optical
sense to investigate the influence of formulations, where only the sand appearance of the liquid mortar.
the sand quality on the application quality was altered, shows that the Formulation 7 (table 2) proves that
and final properties of tile adhesives. properties obtained are almost the use of ground limestone in
In our studies we limited the identical. Sand has the function of a moderate amounts does not harm
number of sands to two very filler in a tile adhesive formulation. the end properties of a tile
different types. Zimmerli sand is a It is therefore to be expected adhesive. Excessive amounts of
highly refined quality with a rather that the influence on the tensile ground limestone, however, have a
narrow particle size distribution adhesion strength remains low. detrimental effect on open time.
(0.1 – 0.3 mm) and a very low The sand with the higher specific
specific surface (< 0.1 m2/g ). In surface required two parts more
6 contrast, Steidle sand has a broader water in order to maintain the
particle size distribution (0 – 0.45 same slip and consistency.
Properties
Rheology
BF 0.5 rpm mPa·s 3,971,000 3,793,000 4,298,000
BF 5.0 rpm mPa·s 557,000 528,000 570,000
BF 50 rpm mPa·s 91,000 84,000 94,000
Slip mm 0.5 0.5 0.5
Tensile adhesion strength
Standard N/mm2 1.16 1.19 1.08
20 min open time N/mm2 1.56 1.59 1.59
30 min open time N/mm 2
1.03 1.27 1.02
Water immersion N/mm 2
0.43 0.61 0.54
Heat aging N/mm 2
0.94 1.00 0.87
Cellulose ethers are among the pronounced thickening effect. determined at 0.5rpm and 50rpm,
most important additives in a tile METHOCEL 10-0350 has a compa- is used.With the exception of the
adhesive formulation.These additives rable viscosity (~10 000 mPa·s) results after hot aging, the tensile
substantially affect application and mode-rately modified, and experi- adhesion results are comparable.
end properties. Cellulose ethers are mental celluose ether XCS Reducing the degree of modification
not only thickeners, controlling 41120.00 is even less modified. In appears to have a positive effect on
water demand and water retention, the test series (Table 3) the water the tensile adhesion after heat aging.
but also through the degree of level was adjusted in order to obtain The tensile adhesion after heat
modification and their rheological approx. 400 000 mPa·s (5.0 rpm). aging represents in many cases the
effect, they determine the tensile Depending on the degree of most critical obstacle to fulfilling
adhesion strength, slip resistance, modification the water demand EN 12004.The slip resistance and
open time and application proper- changed accordingly.The slip the water demand are negatively
ties. resistance decreases with water influenced by a lower degree of
demand, which can be explained by modification. One way out of this
7 The following table demonstrates the lower structural viscosity of the dilemma would be an additive that
the influence of different cellulose liquid mortar. The structural visco- increases the water demand and
ether types on the properties of sity is a measure of how much the slip resistance, without having a
a tile adhesive. viscosity decreases with increasing negative impact on tensile adhesion,
shear rate. As a measure of the especially after hot aging.
Results: METHOCEL 10-0356 is a structural viscosity, the difference of
modified cellullose ether with a the logarithm of the viscosity
Properties
Rheology
BF 0.5 rpm mPa·s 3,750,000 2,780,000 2,100,000
BF 5.0 rpm mPa·s 416,000 396,000 384,000
BF 50 rpm mPa·s 55,000 76,000 76,000
log (0.5 rpm) – log (50 rpm) 1.83 1.56 1.45
Slip mm 0.5 1.5 2.0
Tensile adhesion strength
Standard N/mm2 1.25 1.32 1.45
20 min open time N/mm 2
1.19 1.35 1.25
30 min open time N/mm2 0.69 0.72 0.75
Water immersion N/mm 2
0.68 0.73 0.76
Heat aging N/mm 2
0.34 0.58 0.80
It was found that other, non mulation with the aid of sheet
water-soluble thickeners increase silicates (Pangel S-9) or cellulose
the consistency of cement-based fibres (Arbocel BWW 40) without
tile adhesives, without negative reducing the slip resistance. Even
consequence on the tensile adhe- more important is the fact that the
sion. Sheet-silicates and cellulose tensile adhesion does not deterio-
fibres are such products. rate by the addition of these types
of additives.
Results: Table 4 clearly demonstra-
tes that it is possible to increase the
water demand of a tile adhesive for-
Properties
Rheology
BF 0.5 rpm mPa·s 3,790,000 3,201,000 2,960,000
BF 5.0 rpm mPa·s 594,000 464,000 436,000
BF 50 rpm mPa·s 96,000 79,000 73,000
Slip mm 1.0 0.75 1.0
Tensile adhesion strength
Standard N/mm2 1.19 1.31 1.20
20 min open time N/mm 2
1.69 1.44 1.35
30 min open time N/mm 2
1.27 1.10 1.28
Water immersion N/mm2 0.85 0.96 1.01
Heat aging N/mm 2
0.89 1.22 1.21
Results: Bentone GS, a hectorite the open time and the adhesion
and Optibent CP, a bentonite, have after the heat aging deteriorate.
nearly the same effect on the tensile Pangel S9, a sepiolite has proven to
adhesion properties. Optibent CP be most effective.The thickening
increases the viscosity to a lesser effect is twice as efficient as
degree than Bentone GS. hectorite or bentonite. In practice
Attapulgites, such as Minugel 200 this means that only half the dosage
increase the consistency, but they level is required to reach the same
have a negative influence on tensile viscosity.The tensile adhesion is
adhesion properties. In particular, not influenced and remains high.
Properties
Rheology
BF 0.5 rpm mPa·s 3,600,000 3,974,000 2,690,000 3,290,000
BF 5.0 rpm mPa·s 528,000 598,000 478,000 440,000
BF 50 rpm mPa·s 93,000 100,000 85,000 77,000
Slip mm 1.0 1.0 1.0 0.5
Tensile adhesion strength
20 min open time N/mm2 1.95 1.41 1.90 1.32
30 min open time N/mm 2
0.99 0.48 1.07 0.94
Water immersion N/mm2 0.84 0.74 0.85 0.81
Heat aging N/mm 2
0.90 0.64 0.94 0.79
Table 5:The effects of different sheet silicates on the properties of a tile adhesive.
Redispersible polymer powders are Results: A rather simple base for- 2000, which fulfill the requirements
crucial components of high quality mulation with a low water demand of EN 12004/C2.
tile adhesive formulations.These was used.This explains the relatively
additives substantially increase the low tensile adhesion values obtai- As demonstrated in the previous
tensile adhesion and improve the ned. However, the influence an simple formulation, here too in
flexibility of the adhesive link increased powder level has on the Figure 2 an increase in the polymer
between the tile and the substrate. properties in other formulations, powder addition level shows a clear
This feature is very important can be estimated accordingly. improvement in the standard tensile
especially with difficult substrates Without addition of polymer pow- adhesion, as well as in the tensile
like wood, old tiles and when floors ders the tensile adhesion after heat adhesion after heat aging.
are equipped with floor heating. aging has almost completely collap- Apparently, the addition level of
Redispersible polymer powders also sed.The standard tensile adhesion, polymer powder has no influence
play a key role in tile adhesives as well as the tensile adhesion after on the tensile adhesion after water
meeting EN 12004. heat aging, improves when the level immersion. In this formulation the
10 of polymer powder is increased.This addition of only 2% of DLP 2000
The figure below illustrates the effect is more pronounced with DLP is sufficient to achieve a tensile
effect of two different polymer 2000. adhesion of 1.0 N/mm2 after
powders on the tensile adhesion standard, wet and heat aging.
properties of a tile adhesive. Both When cement of better quality is Figure 3 shows the results of
products are vinyl acetate/ethylene used or if other rheological additives deformation measurements of cured
based. However, DLP 2000 is a (sheet silicates, cellulose fibres) are adhesive strips according to EN
harder polymer with a higher glass added to increase the water 12002. It is remarkable to see that
transition temperature than demand it is possible to achieve the maximum transversal defor-
DLP 210. tensile adhesion values with DLP mation more than doubles with the
2
Tensile adhesion, N/mm2
Standard
Heat aging
1.5
Water imm.
Base formulation:
0.5
0
w/o 2% 4% 6% 2% 4% 6%
DLP
Figure 1: Comparison of two DLP products in a tile adhesive formulation at two addition levels.
Proceeding step by step
Redispersible polymer powder
1.8
Tensile adhesion strength, [N/mm2]
0.8
0.6
11
0.4
0.2
0
Standard Water immersion Heat aging
Base formulation
Deformation (mm)
0
0% 2% 4% 6% 2% 4% 6%
DLP 210 DLP 210 DLP 210 DLP 210 DLP 2000 DLP 2000 DLP 2000
Figure 3: Maximum transversal deformation and maximum force of a tile adhesive formulation containing two different types of polymer powders
Proceeding step by step
Redispersible polymer powder
increasing polymer powder level, The choice of the optimum polymer which also depends on the other
whereas the maximum force powder is important to the overall components of the formulation
remains at a similar level. performance of the tile adhesive (e.g. sand, cement, cellulose ether),
such as open time, standard tensile the redispersible polymer powder
The performance with regard to adhesion, tensile adhesion after must be carefully selected to fit the
maximum deformation and force of specified aging procedures, and formulation.
DLP 210 and DLP 2000 are very rheological properties. Depending
similar. on the property profile desired,
Properties
Density kg/m3 1543 1462 1500 1537
Rheology
BF 0.5 rpm mPa·s 3,132,000 3,713,000 3,324,000 3,587,000
BF 5 rpm mPa·s 445,000 457,000 453,000 467,000
BF 50 rpm mPa·s 71,000 77,000 74,000 75,000
Slip mm 1.2 1.5 1.6 1.0
Tensile adhesion strength
Standard N/mm2 1.21 1.47 1.04 1.20
10 min open time N/mm 2
1.70 1.83 1.73 1.96
30 min open time N/mm2 1.54 1.18 1.38 1.92
Heat aging N/mm 2
0.57 0.39 0.38 0.74
Water immersion N/mm 2
0.18 0.79 0.67 0.69
The test results obtained do not 4 hours. For practical and econo- 1323 requirement of 0.5 – 1.5 ml
only depend on the composition of mical reasons, commercially available water absorption. Slab A absorbs
the tile adhesive, but also on the concrete slabs are used for testing. substantially more water, whereas
quality of the substrate, namely the Slabs fulfilling EN 1323 requirements slab B absorbs practically no water.
concrete slabs and the tiles onto are not available at reasonable cost. This behaviour has serious conse-
which the adhesive is applied.The For the study, we had two qualities quences for the tensile adhesion
quality of the concrete slabs of concrete slab at our disposal. results obtained, as the following
depends on various parameters Neither of the slabs fulfills the EN table demonstrates.
like the nature of the surface, the
absorption behaviour and the Water absorption according
thermal expansion coefficient. to EN 1323
Properties
Rheology
BF 0.5 rpm mPa·s 2,112,000 2,112,000 3,511,000 3,511,000
BF 5 rpm mPa·s 465,000 465,000 447,000 447,000
BF 50 rpm mPa·s 101,000 101,000 71,000 71,000
Tensile adhesion strength
10 min open time N/mm2 1.08 1.56 1.06 1.49
30 min open time N/mm 2
0.10 0.36 0.92 1.45
Heat aging N/mm 2
0.10 0.80 0.43 0.94
Water immersion N/mm 2
0.86 0.90 0.82 0.94
Table 7: Tensile adhesion strength obtained with two types of concrete slabs
Proceeding step by step
Concrete slabs and tiles
Results: The tensile adhesion time can be explained by the lack of The fact, that the results with these
results obtained with the more water retention.The adhesive slabs were lower, only indicates
absorbing concrete slabs (A) are in applied onto the more absorbent tougher test conditions, which
this case lower than with the less concrete slab dries out more until should not diminish the quality of
absorbing concrete slabs (B). Only the tile is inserted.The differences the work described.
the values obtained after the water obtained after heat aging are
immersion remain independent of difficult to estimate and are there- The quality of the tiles influences
water absorption.The largest fore the subject of further investiga- the performance of a tile adhesive in
difference in the results obtained tion.The test results of formulation a similar way to that already seen
with the two different slabs was in 30/31 demonstrates that the with the concrete slabs. In the
tensile adhesion strength after heat C1 classification can also be met following table the influence of fully
aging, where values varied by a without redispersible polymer pow- vitrified tiles and porous tiles (from
factor of two to eight. Hence a der depending on the substrate two different tile producers), on the
correlation between water absorp- used (heat aging value). tensile adhesion, is demonstrated.
15 tion and tensile adhesion strength The data show the influence of
could be established. In all our studies we used concrete different tile types on the adhesion
slab type A. Even though it does not performance using two different tile
The difference in the results obtai- meet the EN 1323 requirements, adhesive formulations. A rather
ned after 10 and 30 minutes open the slab yielded reproducible results. simple tile adhesive formulation
Properties
Tensile adhesion strength
10 min open time N/mm2 1.32 0.91 1.16 1.34 0.93 1.09
30 min open time N/mm 2
0.54 0.39 0.62 0.70 0.52 0.67
Heat aging N/mm2 0.46 0.07 0.11 0.38 0.00 0.03
Water immersion N/mm2 1.15 0.70 1.16 1.07 0.67 1.08
The purpose of this part of the Results:The results from this A medium to strong modification
study was to optimise tile adhesive evaluation allow the following con- of the cellulose ether improves the
formulations to meet a C1T/C2TE clusions, which could be specific to open time particularly.The latter
classification as cost effectively as the raw materials used (Steidle sand, also has a strong influence on the
possible.With the help of a com- CEM I 52.5): water demand, which can be
puter aided experimental design increased by 3% whilst maintaining
software program (JMP) the The low viscosity cellulose ether the slip resistance.The addition
influence of the following parame- (4000 mPa·s) has an advantage in level of DLP 2000 has a great
ters were investigated: nominal open time, where the tensile adhe- influence on the adhesion results
viscosity of the cellulose ether, sion was more than 40% higher. after heat aging.
degree of modification as well as A cellulose ether concentration of
addition level of cellulose ether 0.4% also yielded improved adhesion
and polymer powder. after heat aging (+15%).
17
Impact of formulations parameters on the properties of the tile adhesive:
Water demand
Standard
adhesion
20 min open
time
30 min open
time
Heat aging
Water
immersion
Properties
Density kg/m3 1510 1544 1580 1650
Rheology
BF 0.5 rpm mPa·s 2,905,000 4,318,000 3,206,000 2,985,000
BF 5 rpm mPa·s 445,000 875,000 544,500 352,000
BF 50 rpm mPa·s 82,000 141,000 79,000 49,000
Slip mm 0.5 0.5 0.5 0.5
Tensile adhesion strength
Standard N/mm2 0.92 1.26 1.16 1.37
20 min open time N/mm 2
1.44 1.17 0.98 1.64
30 min open time N/mm2 0.85 0.53 0.99 1.56
Heat aging N/mm 2
0.52 1.17 1.13 1.04
Water immersion N/mm 2
1.09 0.93 1.00 1.08
meeting EN 12004 classifications C1T C1TE+ C2TE C2TE
Raw materials
Cement
Sand
Identification Polymer Bulk density [g/dm3] Ash content [%] MFT [°C] Tg [°C]
DLP 210 PVAc/E 425 10 0 6
DLP 2000 PVAc/E 450 10 2 17
DLP 110 PVAc/VeoVa 450 10 4 22
Experimental
Sheet silicate
Cellulose fibre
Concrete slabs
Tiles
Consistency measurement
Slip fully vitrified tiles (EN 176) 100x100 mm; Heat aging fully vitrified tiles (EN 176) 50 x 50 mm
EN 1308 200g loaded with 50 N for 30 seconds EN 1348 loaded with 20 N for 30 seconds;
slip determined after 20 minutes insertion time within 5 minutes after
mortar application determination of the
Open time porous tiles (EN159) 50x50 mm loaded tensile adhesion strength after 14 days
EN 1346 with 20 N for 30 seconds; insertion time standard climate and 14 days at 70°C
after 10, 20, and 30 minutes tensile
22 adhesion test after 28 days; the insertion Transverse determination of the transverse defor-
time at which the tensile adhesion still deformation mation of tile adhesives and grouts:
exceeds 0.5 N/mm2 is determined EN 12002 The maximum deflection and the maxi
mum stress of a (280 x 45 x 3mm)
Tensile fully vitrified tiles (EN 176) 50x50 mm mortar strip is determined after curing
adhesion loaded with 20 N for 30 seconds; for 14 days in a polyethylene bag and
EN 1348 insertion time within 5 minutes after 14 days at standard climate conditions
mortar application determination of the
tensile adhesion strength after 28 days
Notice: No freedom from any patent owned by Seller or others is to be inferred. Because use conditions and applicable laws may differ from one
location to another and may change with time, Customer is responsible for determining whether products and the information in this document are
appropriate for Customer’s use and for ensuring that Customer’s workplace and disposal practices are in compliance with applicable laws and other
governmental enactments. Seller assumes no obligation or liability for the information in this document. NO WARRANTIES ARE GIVEN; ALL IMPLIED
WARRANTIES OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE ARE EXPRESSLY EXCLUDED.