Kiwa GmbH Polymer Institut Quellenstraße 3 D-65439 Flörsheim-Wicker Tel. +49 (0)61 45 - 5 97 10 www.kiwa.de
Test report P 10430 Testing order:
Testing of the solvent-free epoxy-resin adhesive ASODUR-K4031 in accordance with the test programme in accordance with DIN EN 1504-4 “Products and systems for the protection and repair of concrete structures – Structural bonding”
Customer:
SCHOMBURG GmbH & Co. KG Aquafinstr. 2-8 D-32760 Detmold
Person in charge:
Dipl.-Ing. (FH) N. Machill B. Eng. (FH) S. Schmidt
Period of testing:
September 2016 to June 2017
Date of the test report:
2017-06-08
This test report comprises:
19 pages including Annex 1 1 enclosure of 2 pages
The test results exclusively refer to the tested materials. The publication of the test report in extracts and references to tests for advertising purposes require our written agreement in each single case.
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CONTENTS
1
SUBJECT ........................................................................................................................... 3
2
RECEIPT OF SAMPLES ................................................................................................. 4
3
PREPARATION OF THE TEST SPECIMENS ............................................................ 4
3.1
Mixing of the adhesive....................................................................................................... 4
3.2
Preparation of the test specimens .................................................................................... 4
3.3
Preparation of the composite specimens ......................................................................... 5
4
TESTS................................................................................................................................. 5
4.1
Compressive strength ........................................................................................................ 5
4.2
Shear strength .................................................................................................................... 6
4.3
Open time ........................................................................................................................... 7
4.4
Pot life ................................................................................................................................. 8
4.5
Modulus of elasticity in compression ............................................................................... 9
4.6
Glass transition temperature ............................................................................................ 9
4.7
Coefficient of thermal expansion ................................................................................... 10
4.8
Total shrinkage of structural bonding agents (alternative test method) .................... 12
4.9
Usability and hardening under special ambient conditions ........................................ 13
4.10
Adhesion ........................................................................................................................... 14
4.11 Durability (heat and humidity) ...................................................................................... 15 4.11.1 Thermal cycling ............................................................................................................... 16 4.11.2 Humid environment ........................................................................................................ 17 5
SUMMARY ...................................................................................................................... 18
Enclosure
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SUBJECT The Schomburg GmbH & Co. KG, Detmold, ordered the Polymer Institut to carry out tests on the solvent-free, two-component epoxy-resin adhesive ASODUR-K4031 from the test programme in accordance with EN 1504-4:2005 “Products and systems for the protection and repair of concrete structures – Structural bonding”. In agreement with the customer the following tests from the test programme have been carried out: Overview 1:
Selected tests from the test programme of EN 1504-4
Test
Test specification
Edition
Compressive strength
EN 12190
1998
Shear strength
EN 12615
1999
Open time
EN 12189
EN ISO 9514
2005
Modulus of elasticity in compression
EN 13412
2006
Glass transition temperature
EN 12614
Coefficient of thermal expansion
EN 1770
EN 12617-3
2002
EN 12636
EN 13733
Pot life
Total shrinkage of structural bonding agents (alternative test method) Usability and hardening under special ambient conditions - Low temperature (10°C) - Wet substrate Adhesion Durability (heat and humidity) - Thermal cycling - Humid environment
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RECEIPT OF SAMPLES The samples given in the following overview were delivered to the Polymer Institut. Overview 2: Pos.
Material
ASODUR-K4031
Receipt of samples Component
Batch
Quantity [kg]
A
206409
3 x 4.0
B
3 x 2.0
PREPARATION OF THE TEST SPECIMENS The mixing of the adhesive as well as the preparation of the test specimens has been carried out at standard conditions in accordance with EN 23270.
Mixing of the adhesive The mixing of the adhesive has been carried out in accordance with the mixing ratio given in the following table. Overview 3:
Mixing ratio of the components
Material ASODUR-K4031
Mixing ratio Component A
Component B
The material was dosed in the given mixing ratio and manually mixed by means of a spatula for approx. 3 min until homogenised.
Preparation of the test specimens Immediately after mixing, the adhesive was filled into prism moulds and stripped after a hardening time of 24 hours. Six prisms with the dimensions 40 mm x 40 mm x 160 mm were prepared for testing the compressive strength and the modulus of elasticity. For testing the compressive strength cubes with an edge length of 40 mm were sawed from the prisms by means of wet sawing.
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Preparation of the composite specimens First, prisms with the dimensions 40 mm x 40 mm x 160 mm and cubes with the dimensions 100 mm x 100 mm x 100 mm were sawed from concrete slabs of type MC (0.40) in accordance with EN 1766:2017 by means of wet sawing. Some of the prisms were cut through the centre or at an angle of 60° to the prism axis, so that two identical prism halves were produced. Subsequently, the surfaces of the prisms and cubes to be bonded were roughened by means of blast-cleaning and cleaned under running water by means of a brush. The preparation and storage of the bonded composite specimens is given in the respective sub-clause of the test.
TESTS The tests have been carried out at standard conditions in accordance with EN 23270, if not indicated otherwise.
Compressive strength The compressive strength was determined in accordance with EN 12190 “Products and systems for the protection and repair of concrete structures – Test methods – Determination of compressive strength of repair mortar”. Table 1:
Bulk density and compressive strength
Test specimen No.
Bulk density [kg/dm³]
Compressive strength [MPa]
1.68
73.2
1.69
69.1
1.70
71.4
69.6
5
71.3
6
70.5
Mean value
71.0*
* rounded to 0.5 MPa
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Shear strength The compression shear strength of the compound hardened concrete – hardened concrete was determined in accordance with DIN EN 12615 “Products and systems for the protection and repair of concrete structures – Test methods – Determination of slant shear strength”. Preparation of the test prisms 1. Pre-storage (dry surface): The prism halves with an angle of = 60° to the prism axis have been stored for 48 h at a temperature of (21 2)°C and relative humidity of (60 10) % r. h. 2. Preparation: The adhesive is applied 5 min. after mixing of the components in the specified film thickness of 1 to 2 mm. Directly after application of the adhesive the prism halves were compressed by means of a clamp frame and stored for 24 h. 3. Storage: After 24 hours the test specimens were taken from the clamp frame and hardened for the duration of 7 days at an air temperature of (21 2)°C. The determined measuring values for breaking load, compression shear strength as well as the adhesive bond are summarized in the following table. Table 2:
Breaking load, compression shear strength and type of failure
Test specimen
Test prisms ( = 60°) Mean value Reference test specimens Mean value
[kN] 82.4
Compression shear strength [MPa] 22.3
A 50
79.5
21.5
100
-
86.6
23.4
82.8
22.4
81.0
21.9
91.6
24.8
94.5
25.6
89.0
24.1
Breaking load
Type of failure [%] B C 50
D -
---
Key: A: Cohesion failure within one of the concrete substrates B: Adhesion failure on one of the interfaces adhesive – concrete C: Cohesion failure in the adhesive layer D: Adhesion failure on both interfaces adhesive – concrete
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Open time The open time was determined in accordance with EN 12189 “Products and systems for the protection and repair of concrete structures – Test methods – Determination of open time”. The open time is the maximum time interval between completion of the mixing process of the adhesive and the bonding of the respective surfaces after which the failure in the concrete occurs. Preparation of the test prisms 1. Pre-storage: The prism halves have been stored for 48 h at a temperature of (21 2)°C and relative humidity of (60 10) % r. h. 2. Preparation: The adhesive is applied on one prism half 10 min. after mixing of the components in the specified film thickness of approx. 2 mm. After 40, 55, 70, 85, 100 and 115 min. both of the prism halves were joined and loaded with a clamping force of (320 ± 20) N until testing. 3. Storage: The test specimens have been stored in the clamping apparatus for the duration of 7 days at an air temperature of (21 2)°C and relative humidity of (60 10) % r. h. Test and result: During the four point bending test after 7 d the vertical load was applied on the test specimens clamped in the clamping apparatus until failure by means of a traverse distributing the load. The open time results as soon as the failure occurs in the adhesive joint but not in the concrete. Table 3:
Breaking load and type of failure Type of failure / failure level [%] A B 100 -
Time period after mixing
[min] 40
[kN] 2.85
55
2.78
70
2.16
85
2.27
2.12
115
2.22
60
40
Test piece No.
Key: A: Cohesion failure concrete B: Adhesion failure between adhesive and concrete
The open time is 100 min.
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Pot life The pot life was determined based on EN ISO 9514:07-2005 “Paints and varnishes – Determination of the pot life of multicomponent coating systems – Preparation and conditioning of samples and guidelines for testing” on the material Kemko 068 in compliance with the following test conditions: Test device: Evaluation: Measuring interval: Homogenisation: Test volume: Temperature development: Number of determinations:
OMB-DAQ-56, Omega with thermal element Fe-CuNi Dasy-Lab 6.0 - Software 10 s 1 min mixed with wooden spatula 100 cm³/ can diameter 6,5 cm; deviating from the standard Adiabatic, in the thermally insulated reactor 2
The following parameters were determined: Pot life Time between the mixing at the respective start/initial temperature and reaching an increase of 15 K Reaction time Interval until reaching the maximum temperature (Tmax) of the mixture Maximum temperature of the mixture The determined pot life is a laboratory value, which can deviate from the actual processing time. The determined single (SV) and mean values (MV) are given in the following table, the temperature/time diagram is given in figures 1 to 3 of the enclosure. Table 4:
Start temperature
Pot life [min]
Maximum temperature [°C] SV MV
[°C]
SV
MV
10
47 ; 50
48
39 ; 39
21
45 ; 44
44
30
23 ; 22
23
SV = Single value / MV = Mean value
Reaction time [min] SV
39
119 ; 125
122
47 ; 46
47
92 ; 90
91
70 ; 72
71
51 ; 51
51
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Modulus of elasticity in compression The modulus of static elasticity was determined in accordance with EN 13412 “Products and systems for the protection and repair of concrete structures – Test methods – Determination of modulus of elasticity in compression”. Parameters: test machine: loading rate: displacement transducer: upper test stress:
Schenk-Trebel 600 kN test press 10 N/mm²/s DD1, measuring length 100 mm 14 N/mm²
The results are given in the following table. Table 5:
Modulus of static elasticity in compression
Test piece No. 1 2 3
Stress [MPa]
Compression [-]
23,13
0,617
0,62
0,133
0,470
0,053
0,519
0,072
Modulus of e * [MPa]
Mean value:
4.700 5.400 5.000 5.000
* Rounded to 100 N/mm²
Glass transition temperature The glass transition temperature of the hardened material was determined at an age of 7d in accordance with EN 12614 “Products and systems for the protection and repair of concrete structures – Test methods – Determination of glass transition temperatures of polymers” in compliance with the following test conditions: device: heating rate: cooling: sample holder: initial weight of the sample: atmosphere:
DSC 200 by Netzsch Gerätebau GmbH -10 °C to 150°C with 20 K/min free cooling aluminium cup 18.6 mg N2, pureness 4.0, 50ml/min
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The result is given as the centre temperature in the following table. Table 6:
Figure 1:
Glass transition temperature after 7d of hardening at 21 2 °C Material
Glass transition temperature [°C]
40.7
Coefficient of thermal expansion The coefficient of thermal expansion t was determined using the pushrod dilatometer by the Netzsch company in accordance with EN 1770 “Products and systems for the protection and repair of concrete structures – Test methods – Determination of the coefficient of thermal expansion” at an age of 7 d after storage B. Information on the horizontal pushrod dilatometer DIL 402 ES: sample holder: quartz push rod: quartz contact pressure: 5 cN inductive displacement transducer measurement L: temperature measuring range: -40 °C to +100 °C atmosphere: nitrogen
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For this, a test specimen 5 mm x 5 mm x 50 mm was cut from a prism. Subsequently, the measurement was carried out. The result is given in the following table and figure. Table 7:
Coefficient of thermal expansion after 7 d of hardening at 21 2 °C -20.0 ≤ T ≤ +23.0 °C
Coefficient of thermal expansion t 36.9 x 10-6 /K
-20.0 ≤ T ≤ +40.0 °C
41.7 x 10-6 /K
+23.0 ≤ T ≤ +40.0 °C
53.8 x 10-6 /K
Temperature range
Figure 2: Coefficient of thermal expansion
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Total shrinkage of structural bonding agents (alternative test method) The total shrinkage of the adhesive was determined in accordance with EN 12617-3 “Products and systems for the protection and repair of concrete structures – Test methods – Part 3: Determination of early age linear shrinkage for structural bonding agents”. Directly after mixing, the adhesive was filled into a steel mould in accordance with figure 1 of the standard mentioned above, the front surfaces were declamped from the latching and have been hardened for 48 hours at standard conditions in accordance with DIN EN 23270. During the hardening time the change in length of the adhesive as well as the temperature have been recorded by means of sensors. The graphic illustration of the results of shrinkage over time as well as the temperature profile are given in the following figure.
Figure 3: Results of shrinkage over time The total shrinkage at the end of the test was 0.072 %.
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Usability and hardening under special ambient conditions The test of the usability and hardening under special ambient conditions for the test method “hardened concrete – hardened concrete” has been carried out in accordance with EN 12636 “Products and systems for the protection and repair of concrete structures – Test methods – Determination of the adhesion concrete to concrete”. Preparation of the composite specimens 1. Pre-storage: Wet substrate The test specimens have been stored for the duration of 48 h under water at room temperature. Prior to application of the adhesive the surface to be bonded was put up in vertical position for the duration of 15 min at a temperature of (21 ± 2) °C and relative humidity of (60 ± 10) %, in order to drain off the free water. Limit temperature 10°C The prism halves have been stored for 48 h at a temperature of 10°C and relative humidity of (75 10) % r. h. 2. Preparation: The adhesive is applied 5 min. after mixing of the components. Directly after the application of the adhesive both of the prism halves were compressed by means of a clamp frame, so that an adhesive layer of approx. 1 – 2 mm thickness was achieved. 3. Storage: The test specimens have been stored and hardened without clamp frame for the duration of 7 days at a temperature of (21 2)°C. Test and result: After 7 d, during the four point bending test a vertical load is applied until failure by means of a traverse distributing the load. The following tables list the determined measuring values for the breaking load as well as the type of failure. Table 8: Test piece No.
Test method hardened concrete-hardened concrete – Wet surface Breaking load
[min]
[kN]
C
2.71
100*
2.80
2.19
1 2
Type of failure [%]
Adhering after mixing
3 Mean value * Concrete failure near the surface
2.7
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Table 9: Test method hardened concrete-hardened concrete – Limit temperature 10 °C Test piece No.
1.44
2.14
2.53
1 2 3 Mean value
2.0
Key: A: Cohesion failure in the adhesive layer B: Cohesion failure in the concrete C: Adhesion failure between adhesive and concrete
Adhesion The test of the adhesion for the test method “hardened concrete –hardened concrete” has been carried out in accordance with EN 12636 “Products and systems for the protection and repair of concrete structures – Test methods – Determination of the adhesion concrete to concrete”. Preparation of the composite specimens 1. Pre-storage: The prism halves have been stored for 48 h at a temperature of (21 2)°C and relative humidity of (60 10) % r. h. 2. Preparation: The adhesive is applied 5 min. after mixing of the components. Directly after the application of the adhesive both of the prism halves were compressed by means of a clamp frame, so that an adhesive layer of approx. 1 – 2 mm thickness was achieved. 3. Storage: The test specimens have been stored for the duration of 7 days at a temperature of (21 2)°C and relative humidity of (60 10) % r. h. Test and result: After 7 d, during the four point bending test a vertical load is applied until failure by means of a traverse distributing the load. The following tables list the determined measuring values for the breaking load as well as the type of failure.
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Table 10:
Breaking load and type of failure
3.16
3.35
2.83
3 Mean value
Key: A: Cohesion failure in the adhesive layer B: Cohesion failure concrete C: Adhesion failure between adhesive and concrete
4.11
Durability (heat and humidity) The durability (heat and humidity) was determined in accordance with EN 13733 “Products and systems for the protection and repair of concrete structures – Test methods; Determination of the durability of structural bonding” after thermal cycling and storage in humid environment. Preparation of the composite specimens 1. Pre-storage: The concrete cubes have been stored for 48 h at a temperature of (21 2)°C and relative humidity of (60 10) % r. h. 2. Preparation: The adhesive is applied 5 min. after mixing of the components in the specified film thickness of approx. 1 mm on one surface of two cubes in each case. Subsequently, the composite specimens were joined. 3. Storage: The composite specimens have been stored for the duration of 28 days at a temperature of (21 2)°C and relative humidity of (60 10) % r. h. Carrying out the test The test has been carried out with the following parameters: 5000 kN test press by the MAN company in accordance with Test machine: EN 12390-4 In accordance with figure 1a and 1b of EN 13733 Test apparatus:
Test rate:
(60 ± 20) kN/min
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4.11.1
Thermal cycling The exposure has been carried out in accordance with sub-clause 5.1 of the standard mentioned above in a programmable climate chamber with the following cycle:
333 minutes storage in air at T = (-25±2)° C 27 minutes heating in air at T = (+55±2)° C 333 minutes storage in air at T = (+55±2)° C 27 minutes cooling in air at T = (-25±2)° C
The cycle mentioned above has been repeated 50 times. Subsequently, the test specimens have been reconditioned for a minimum of 24 hours in the climate (21±2)° C/(60±10)% r. h. (TWB01-3). The conditioning for comparison purposes has been carried out in accordance with EN 13733 sub-clause 6.1 “General” in the climate (21±2)° C/(60±10% r. h.) (reference 1-3). Table 11:
Breaking load and type of failure – Thermal cycling Compression shear load
Shear stress
[MPa]
left
right
TWBO 1
16.2
0.8
70 AK / 30 KB
TWBO 2
83.2
60 AK / 40 KB
100 AK
TWBO 3
82.5
50 AK / 50 KB
Test piece
mean value:
Failure pattern [%]
3.0
Reference 1
201.0
10.0
10 AK / 90 KB
20 AK / 80 KB
Reference 2
100.4
5.0
Reference 3
210.1
10.5
12.8
Key: AK: Adhesion failure between adhesive and concrete KK: Cohesion failure adhesive KB: Cohesion failure concrete
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4.11.2
Humid environment The exposure has been carried out in accordance with EN 13733 sub-clause 5.2 “humid environment” in a climate chamber with the following parameters:
climate: duration:
(+40±2)°C / (95±5) % r. h. 6 months
Subsequently, each test specimen has been reconditioned for a minimum of 24 hours in the climate (21±2)° C/(60±10% r. h.). After the exposure to the climate mentioned above the test of the shear stress has been carried out. The conditioning for reference purposes has been carried out in accordance with EN 13733 sub-clause 6.1 “General” in the climate (21±2)°C / (60±10% r. h.). Table 12:
Breaking load and type of failure – Humid environment Failure pattern [%]
Compression shear load
Left
Right
FWU 1
133.4
6.7
10 KK / 90 KB
FWU 2
203.3
10.2
100 KB
FWU 3
221.1
11.1
40 AK / 60 KB
9.3
--10 AK / 90 KB 20 AK / 80 KB
203.9
161.4
8.1
171.4
8.6
9.0
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SUMMARY The Schomburg GmbH & Co. KG, Detmold, ordered the Polymer Institut to carry out tests on the solvent-free, two-component epoxy-resin adhesive ASODUR-K 4031 from the test programme in accordance with EN 1504-4:2005 “Products and systems for the protection and repair of concrete structures – Structural bonding”. A summary of the test results and a comparison to the requirements of EN 1504-4 is given in Annex 1.
Flörsheim-Wicker, 2017-06-08 The assistant head of the institute
The person in charge
Dipl.-Ing. (FH) N. Machill
B. Eng. (FH) S. Schmidt
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Annex 1 Comparison of the results with the requirements of EN 1504-4, Table 3.2 Performance characteristic
Unit
Result
Requirement
71.0
≥ 30
≥6
Declared value 20 %
Pot life Start temperature: 10 °C 21 °C 30 °C
[min] 48 44 23
Declared value
5,000
≥ 2,000
≥ 40
36.9 x 10-6 41.7 x 10-6 53.8 x 10-6
αT ≤ 100 x 10-6
[%]
0.072
ssoll ≤ 0,1 %
Usability and hardening under special ambient conditions - Wet substrate
- Limit temperature 10°C
100 % failure in the concrete 100 % failure in the concrete
Failure in the concrete
Adhesion
100 % failure in the concrete
Cohesion failure in the concrete
- Thermal cycling
- Humid environment
Glass transition temperature Coefficient of thermal expansion Temperature range: -20,0 ≤ T ≤ +23,0 °C -20,0 ≤ T ≤ +40,0 °C +23,0 ≤ T ≤ +40,0 °C Total shrinkage of structural bonding agents
[1/°C]
Durability (Heat and humidity) The compression shear load at failure shall not be lower than the tensile strength of the hardened concrete. *
* Surface tensile strength in accordance with EN 1766 for the reference concrete type MC (0,40) = 3,0 N/mm²
Page 1 of the enclosure to the test report P 10430
Processability at a start temperature of 10°C
Figure 2:
Processability at a start temperature of 21°C
Page 2 of the enclosure to the test report P 10430
Figure 3:
Processability at a start temperature of 30°C