Report

about the

Artificial weathering with fluorescent UV lamps according to ISO

11507, method A for different coatings on sandstone

Order Number: 72013209

Customer: NANO4LIFE EUROPE®

Vouliagmenis Ave. 318
Ag. Dimitrios - 173 43
ATHENS
GREECE

Contractor: Polymer Service GmbH Merseburg

Business Area
Plastics Testing and Plastic Diagnostics
Prof. Dr. rer. nat. habil. W. Grellmann
Geusaer Str., Building Fo 131
D-06217 Merseburg
Tel.: 03461 462777
Fax: 03461 462592
E-Mail: wolfgang.grellmann@iw.uni-halle.de
Internet: www.polymerservice-merseburg.de

Processor: Dr.-Ing. Marcus Schoßig

Tel.: 03461 46 2874
E-Mail: marcus.schossig@psm.uni-halle.de

This report contains -6- pages inclusive first page as well as -1- appendix.

Address: Bank Account: Management Board:

Polymer Service GmbH Merseburg Dresdner Bank Merseburg HRB-Nr.: 13391 Prof. Dr. W. Grellmann
Geusaer Str., Building. Fo 131 Bank Code: 800 800 00 USt-IdNr.: DE213194336 Prof. Dr. B. Langer
D-06217 Merseburg Account Number: 08 116 301 00 St.-Nr.: 112/115/00486
Germany BIC/SWIFT: DRES DE FF 800
IBAN: DE 03800800000811630100
 Polymer Service GmbH Merseburg
An-Institut at the Martin-Luther University Halle-Wittenberg

Content

1 Problem, Materials and Exposition ................................................................................... 3

2 Experimental Details ........................................................................................................ 4

2.1 Artificial Weathering according to ISO 11507, Method A – Fluorescent

UV lamps and Water ......................................................................................... 4

2.2 Determination the Contact Angle according to DIN 55620-1 and DIN 55620-2 . 6

3 Results ............................................................................................................................. 7

4 Literature ......................................................................................................................... 12

Appendix

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 Polymer Service GmbH Merseburg
An-Institut at the Martin-Luther University Halle-Wittenberg

1. Problem, Materials and Exposition

For the examinations, the customer provided sandstone materials with two different coatings;
NANO4-STONE and AG INDUSTRIES. The objective is the assessment of the aging behavior according
to ISO 11507, method A. Figure 1 shows a photograph of the sandstone materials in the used
specimen holders before the weathering started.

Figure 1: Photograph of the sandstone materials mounted on the used specimen holders

2. Experimental Details

2.1 Artificial Weathering according to ISO 11507, Method A – Fluorescent UV lamps and
Water [1]

INTRODUCTION
For many products, it is necessary to be weather-resistant mainly to UV radiation. However, under
“weather-resistant” should be understood the fulfillment of the requirement profile of the prod-
ucts. For example, an aging effect can be existent, if products show optical changings like discol-
orations or loss of gloss. These effects are a clear fault for the customers. The term aging is defined
in the standard DIN 50035 as ‘the accumulation of irreversible chemical and physical reactions in
a materials’ [„die Gesamtheit aller im Laufe der Zeit in einem Material irreversibel ablaufenden
chemischen und physikalischen Vorgänge“] [2].
During the use of technical products, a natural weathering as well as a weathering behind window
glass over several years can be occur. Based on the dependency of the results on the weathering
location, this means from the local climate, the season as well as the position on the earth, the
artificial weathering has significant benefits for the assessment of the weatherability. Predictions,
which are independent of the location, are possible by a constant and reproducible irradiance,
temperature, and moisture as well as condensation or spray cycles.
The most important thing for the choice of a suitable test method is an adequate simulation of
the solar radiation by the used radiation source. This is realized by xenon-arc lamps through the
usage of proper filters, wherefore the xenon-arc lamps are preferred for the simulation of the
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 Polymer Service GmbH Merseburg
An-Institut at the Martin-Luther University Halle-Wittenberg

global irradiance. The photochemical effective UV and short-wavelengths range is important for
the aging of polymers. For such investigations, fluorescent UV lamps are used.
For the simulation of the UV radiation in the QUV/ SPRAY (Co. Q-LAB CORPORATION, USA), fluorescent
UV lamps according to ISO 11507 were used. The radiation emission in the UV range, this means
below 400 nm, is minimum 80 % of the total emission. Typically, fluorescent UV lamps are used
with a radiation content of less than 2 % below 300 nm and an emission peak at 340 nm (UV-A-
340, Type II) [1]. The required spectral distribution is realized through a proper selection of the
phosphor coating on the inner surface of the lamps and the used glass type. Figure 2 shows the
irradiance of direct sunlight in comparison to the UV radiation of the used UV-A-340 lamp. The
solar energy barrier (UV cut-off) is 295 nm and the radiation maximum is 340 nm.

Figure 2: Comparison of the spectrum of the fluorescent UV lamp UV-A-340 (Type II) with direct sunlight [3]

EXPERIMENTAL DETAILS
By the method A – according to ISO 11507 – the specimens were exposed to UV radiation, tem-
perature and condensation phase with distilled water to reproduce weathering effects, which can
appear in reality and for the use of the products typical environments (UV radiation) in the mate-
rial. The test condition are listed below and Figure 3 shows the used accelerated weathering tester
QUV/SPRAY.

Table 1: Test conditions according to ISO 11507, method A

Lamp type UV-A-340 (Type II)

Irradiance El 0.76 W · m-² · nm-1
Black panel temperature 60°C ± 3°C
Black panel temperature during condensation 50°C ± 3°C
Method A:
Dry phase 4 hours
Condensation 4 hours (UV lamps off)
Exposure time 3500 h

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 Polymer Service GmbH Merseburg
An-Institut at the Martin-Luther University Halle-Wittenberg

Figure 3: Accelerated weathering tester QUV/SPRAY and water treatment plant type ELIX 15

2.2 Determination the Contact Angle according to DIN 55620-1 and DIN 55620-2 [4, 5]

The determination of the contact angle q according to DIN 55660-2 took place with distillated
water as test liquid. The measurements were realized with the testing device DSA100 TROPFENANA-
LYSE-SYSTEM (DROP ANALYSIS SYSTEM) of the company KRÜSS GmbH, Germany. For the determination
of the contact angle q, the angle to the baseline, which arise to the tangent on the drop contour
at the three-phase point, was used. This can be seen schematically in Figure 4.
The determination of the contact angle q was repeated every 500 h in the center of the specimens.
The test conditions are shown in Table 2.

Figure 4: Schematic representation of the contact angle measurements; 1 – three-phase point, 2 – liquid, σl – surface energy
of the liquid, σS – free surface of the solid state surface, σSl – interface energy between solid state surface and liquid.
q – contact angle [4]

Table 2: Test conditions for the measurements of the contact angle

Test liquid: distillated water

Drop capacity: 4 µl
Number of drops: 10
Manner of contact angle measurements: static
Numerical method (measurement range):
Young-Laplace equation 20° till 110° and 110° till 180°
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 Polymer Service GmbH Merseburg
An-Institut at the Martin-Luther University Halle-Wittenberg

3. Results

The contact angle q was measured every 500 h within a period of 3500 h. A graphical representa-
tion of the result is shown in the following figure and a tabular listing can be found in appendix 1.
Figure 5 shows the dependence of the values determined for the contact angle q on the exposure
time for the coatings NANO4-STONE and AG INDUSTRIES on sandstone. Both coatings show a contrary
behavior. For the coating AG INDUSTRIES, an initial value of 130.8° and after an exposure time of 500
h of 50.6° was determinable. A determination of the contact angle after further 500 h was not
possible, because the contour of the drop was not stable enough for a reliable measurement. The
coating NANO4-STONE shows a different behavior shows, which is characterized by an increase in
the contact angle q from 131.6° to 147.9° after an exposure time of 3500 h. A possible interpre-
tation of this behavior is the chemical post-crosslinking of the coating.

Figure 5: Comparison of the coating NANO4-STONE and AG INDUSTRIES on the weathering stability; eot … end of test

4. Literature
[1] ISO 11507 (2007-05): Paints and varnishes – Exposure of coatings to artificial weathering – Exposure to fluorescent UV
lamps and water
[2] DIN 50035 (2012-09): Terms and definitions used on ageing of materials – Polymeric materials
[3] Fowler, S.: Spectral power distribution data for UVA-340 and UVA-351 lamps used in the QUV, and Daylight-Q and
Window-Q filters used in the Q-Sun. Q-Lab Corporation, Personal Communication September 6, 2011.
[4] DIN 55660-1 (2011-12): Paints and varnishes – Wettability – Part 1: Terminology and general principles
[5] DIN 55660-2 (2011-12): Paints and varnishes – Wettability – Part 2: Determination of the free surface energy of solid
surfaces by measuring the contact angle

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 21.11.2013
Appendix 1
Page 1/1
Mean value of the contact angle θ (°); Weathering with UV fluorescent lamps according to ISO 11507, method A
Material Coating Initial value SD 500 h SD 1000 h SD 1500 h SD 2000 SD 2500 SA 2000 SD 2500 SA
NANO4-STONE 131,6 1,9 151,8 0,7 151,7 0,8 146,7 4,5 157,0 5,5 147,9 3,5 153,7 8,2 155,5 5,5
Sandstone
AG INDUSTRIES 130,8 1,4 50,6 1,7 sink in sink in, 2 s (eot)