Q Lab Correlación Entre ASTM D 7869 e Intemperismo Exterior

ASTM D7869: A New Xenon-Arc
Accelerated Weathering
Standard with Improved
Outdoor Correlation
Watch Webinar Stream
Andy Francis, Q-Lab Corporation
ASTM D7869 1 We Make Testing Simple

Why Do Weathering Testing?
OR
High gloss and color integrity
Fading, cracking, peeling
Weathering testing can mean the difference between

happy customers and … the customer on the right

Why Do Weathering Testing?
OR
High gloss and color integrity Gloss loss and color fade
Weathering testing can mean the difference between

happy customers and … the customer on the right

Weathering Testing
• Manufacturers & coatings companies are always
introducing new systems
• Customers may require up to 5 Years natural
outdoor weathering
• Accelerated weathering used to shorten
development & approval time
Weathering testing provides crucial information

about materials’ outdoor performance!
Accelerated
Laboratory Weathering

Types of Accelerated
weathering tests
Pass/fail
– Quality Control; Qualification ; R&D
– Most accelerated weathering
Comparative
– Usually rank-ordering
– Key is to correlate to outdoor
Service life prediction

– Material-specific
– Need lots of indoor/outdoor data - very difficult!

weathering tests
Pass/fail
Comparative


weathering tests
Pass/fail
Comparative


Service Life Prediction -
Challenges
• Requires vast amounts of data
• Not currently practical

– Has not been tested or shown to be
successful with available commercial
coating systems
• Shows promise for the future more for

OEM’s than international standards

weathering tests
Pass/fail
Comparative


Accelerated Lab Weathering to
Generate Comparative Data
• Replicate material degradation

observed outdoors
• Do it faster than outdoors!
How can we do this?

Historical Test Standards
• Xenon arc’s light sources have been used for many
years - accurate reproduction of full-spectrum sunlight
• Hardware-based “102/18” light/light+spray standards

were the first widely-used weathering standard tests
– Almost 100 years old but still in use
– Most common example is ISO 4892-2
– Not realistic!
• SAE J2527 became the “state of the art” in 1980’s

– Research into primary stressors (light, water, heat)
– Replicated gloss loss seen in Florida exposures

Issues with SAE J2527
• Standard was well-researched but did not match

real-world weathering factors
– Light spectra
– Moisture delivery
• As a result, it does not adequately predict

Florida outdoor field failures
– Chemical change (Photo-oxidation, water-based effects)
– Physical change (Cracking, Blistering, Delaminating)

Taking the Next Step:
ASTM D7869
• Outdoor weather data collected to understand real-world
weather conditions: light, heat, and water
• Outdoor weathering test dataset collected to provide

basis for correlation
• Accelerated test cycle developed to match those real-

world conditions and degradation mechanisms
• Variety of materials and failure modes evaluated with

accelerated testing to verify validity of test

Collecting outdoor
weather data
Laying the groundwork for a new
accelerated test

Outdoor weather data
Approach: collect outdoor weather data to better
understanding the forces of natural weathering:
• Sunlight
• Heat
• Water
Goal: Obtain suitable body of field data to

develop the Accelerated laboratory test
Outdoor Weather Data
Collection Sites
• Weather Station Installed at

Bayer Site Jacksonville, FL
– 2004 to 2007
• Moved to Homestead, FL
(Q-Lab)
– 2008 to 2014

Outdoor Weather
Data Collected
• Solar Radiation (Sunlight)
• Temperature
– Air, Black Panel, Relative Humidity and Dew Point
• Wind
– Speed and Direction
• Rain
– Amount, Duration, Rate Accumulation
• Panel Weight
– Wetness, Dew Events and Rain Events

Outdoor Weather
Water Data Measurements
• Mass of panel measured

every 5 min
– Panel + Water
• Calibrated regularly
• Care taken to ensure no

animal or bird influence
• Able to see rain vs dew +

water-uptake

Water on Test Panels
Rain Dew

Dew on Painted Panels
30
C
25
Grams Water on Panel
20
B
E
15
10
D
5
Wind Noise
A
0
Day 1 Day 2 Day 3 Day 4 Day 5

Developing a Library of
Outdoor Weathering Data
Driving towards correlation

Outdoor Testing
Sample selection
• Sample set includes both
common field failures & controls
• 106 Combinations Prepared

– 4 colors: Black, White, Blue, Red
– Waterborne & Solventborne Base
– Solventborne Clear
– Different layering systems
– With and without Stabilizers
• All Samples prepared by one lab

Outdoor Testing
Test Protocol
• Testing conducted per SAE J1976
• Evaluations every 6 months
• Exposure times
• Full Set Summer 2006
• Partial Set Summer 2007
• Expose Until Failure

Developing the
ASTM D7869 Accelerated
Laboratory Test Cycle
Using outdoor weather characteristics
to guide accelerated testing

Learnings from Outdoor for New
Accelerated Weathering Test
• Global benchmark location: South Florida
• Light intensity: use higher-intensity light with

correct spectrum to increase acceleration
• Heat: Keep temperatures realistic, at or below

service
• Time of wetness: Increase! Mimic real-world

behavior - panels wet 12+ hrs/day in Florida
• Water spray: Never spray panels during light step;
it never rains when sun is shining brightly!

Sunlight
• Explored different light sources
• Explored different optical filters
• Accelerated outdoor weathering

(Q-TRAC) provided tantalizing
results
• Better match to sunlight just

might work, but be careful …

The wrong light source gives
the wrong results!
Borosilicate filtered
xenon arc Florida
Peters/Misovski/Roberts/Lemaire/Fischer

Accelerating irradiance
8
Atlas
CIRA/SL Q-Lab Polyester/Urethane
7 Xenon Daylight-Q
Atlas B/B Xenon
Q-Lab Daylight B/B
6 Q-TRAC
No available filters accurately
5
reproduced photooxidation!
∆(a/b)
QUV UVA340
4 FL
SUPRAX
3
Q-Lab Q/B Xenon
2 AZ
SEPAP
1
Atlas Q/B Xenon
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
Peters/Misovski/Roberts/Lemaire/Fischer
∆(c/d)

Accelerated Light Source
• Development team sought a light source with a
better match to the solar spectrum
• Result: a new optical filter now commercially
available from all major equipment
manufacturers
– Daylight – F (Q-Lab)
– Right Light (Atlas)
• Produces more realistic results

– Allows higher irradiance, better acceleration

New Optical Filters
Very good match to sunlight, ability to accelerate with higher irradiance

New Optical Filters
Very good match to sunlight, ability to accelerate with higher irradiance

Heat
High temperature serves primarily

to accelerate water uptake. Two
key guiding principles:
1. Do not exceed maximum service

temperature
2. Use realistic temperatures to

increase correlation

Water contributes to material
degradation in many ways
• Plasticization – reduced modulus
• Swelling – induced stresses due to differential stresses
• Blistering – localized swelling and rupture
• Adhesion – accumulation of water at interface, breakdown

of interfacial bonds.
• Mass transport – movement of small molecules and

reaction products through film.
• Mass loss – removal of film (degradation products) from

surface of the coating due to erosion.

Water
• Establish maximum amount painted
panel can hold
• Establish minimum amount of water

that must reach the specimens
• Determine if accelerated weathering

devices can produce enough water
• Determine Repeatability &

Reproducibility

Water Delivery Calibration:
Sponge Test
• Can be used in both flat array &
rotating drum tester architectures
• Same size & type of sponge in same

holder type used in both machines
• Results were Repeatable &

Reproducible

Sponge Water Calibration Tests
Rotating Drum Flat Array
Shielded sponge holder

Connecting Accelerated Test to
Outdoor Weather Data
• Needed to better match sunlight spectrum
– New optical filter, increased intensity
• Test temperatures need to be reasonable

– Realistic temperatures chosen, below maximum
• Panels were wet longer that commonly believed

– Water delivery calibration system devised
This data helped construct an accurate model for use in

developing an accelerated test method
Development of ASTM
D7869 Test Cycle

Test Development
• Many years of experimentation

– 1st group: BASF, Bayer, Ford, Q-Lab
– 2nd group: Honda, Boeing, Atlas
• Dozens of different approaches
• Multiple runs of final test to ensure

repeatability & reproducibility

Outdoor Light and Water
Typical Florida Daily Cycle
Light Intensity
Panel Water
Content
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Irradiance
SAE J2527
Water Spray Not a Good Match with Outdoor Weather
1.0
0.9
Irradiance (W/m2/nm @340nm)
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Outdoor Light and Water
Typical Florida Daily Cycle
Light Intensity
Panel Water
Content
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Irradiance
ASTM D7869
Water Spray Reproducing Natural Weather Cycles
1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Irradiance
ASTM D7869
Water Spray Deep Water Penetration
1.0
0.9
0.8
0.7
0.6
Deep Water
0.5
Penetration
0.4
0.3 Adhesion,
Blistering,
0.2
Diffusion
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Irradiance
ASTM D7869
Water Spray Separating Water and Light
1.0
0.9
0.8
0.7
0.6
No spray
0.5
during light
0.4 steps
0.3
Avoids
unrealistic
0.2
0.1 failures
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Irradiance
ASTM D7869
Water Spray Thermal Cycling
1.0
Cyclic Stresses (cracking)
0.9 Surface Erosion (gloss)
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

ASTM D7869
Comparison to SAE J2527
• In a 24 hr period, SAE J2527 uses more water
than ASTM D7869, but …
– Never delivers enough water at one time
– Sprays water during the light cycle causing unrealistic
failures with modern coatings
• Fundamentally two different test cycles

– As different as 102/18 and SAE J2527

ASTM D7869
Step-by-Step

Irradiance
ASTM D7869
Water Spray Step 1
1.0
0.9
0.8
0.7
0.6
0.5 Step 1
0.4
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Step 1 240 min Dark + Spray
Air = 40°C RH = 95%+
Purpose: Reproduce Water Uptake

equal to normal night in Florida
• Close to total saturation
• Water uptake in Florida can exceed 5% of
coating volume, typical around 3.5%
• If not enough water test will fail to produce
realistic degradation
• More water uptake is OK, no negative effect
Air = 40°C RH = 95%+
Degradation Caused by Water Uptake

• Cracking
• Loss of inter-coat adhesion
• Delamination
• Loss of low molecular weight materials:
stabilizers, surfactants, acid catalysts.
• Gloss Loss
• Chalking
Air = 40°C RH = 95%+
Why 40oC Temperature?

• Higher temperature only occurs outdoors after
dry-off, as sun warms coating.
• Temperature less then 40°C makes water
uptake happen too slow.
• Water uptake at 40°C is twice as fast as 25°C
• Not so hot as to cause unnatural heat effects.

Air = 40°C RH = 95%+
Why 240 min (4 hours) of Spray?

• Florida wet temperatures are 20°-25°C
• Florida wet times are 8 to 16 hours.
• 4 hours at 40°C produces same water uptake
as longer, cooler Florida wet periods.
• Most outdoors wet time is at night so this
step has no irradiance
Irradiance
ASTM D7869
Water Spray Step 2
1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2 Step 2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Step 2 30 min Light 0.40 W/m2
BP = 50°C Air = 42°C RH = 50%
Purpose: Totally Remove Absorbed Water
• Sun completely dries coating by mid-morning

• Low irradiance, 0.40 W/m2, because sun is not
very bright by mid-morning
• 30 min is sufficient time to dry the coating

BP = 50oC Air = 42oC RH = 50%
Why 50 oC?
• Sun completely dries coating before specimens

get hotter than 50 oC
• Hotter temperature can cause unrealistic
cracking and micro-cracking, caused by coating
drying too fast

BP = 50oC Air = 42oC RH = 50%
Why 50% RH?

• Must control RH. Different RH’s will cause
different rates of drying - 50% produced most
realistic results
• Higher RH would take too long for dry-off
• Lower RH causes unrealistic failures

Irradiance
ASTM D7869
Water Spray Step 3
1.0
0.9
0.8
0.7
0.6
0.5
0.4 Step 3
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

BP = 70°C Air = 50°C RH = 50%
Purpose: Simulate Effects of

Bright Sunlight
• Mostly surface effects. Light does not penetrate
into the bulk polymer like water does.
• Photo-oxidations
• Gloss Loss
• Color Change
• Micro-cracking
BP = 70°C Air = 50°C RH = 50%
Why 0.80 W/m2/nm irradiance?

• Produces realistic accelerated aging
• Higher than maximum irradiance of noon
midsummer sunlight (~0.68 W/m2)
• Most sunlight exposure is lower than
0.68 W/m2
• Data shows 0.80 W/m2 was highest irradiance
that produced realistic degradation

BP = 70°C Air = 50°C RH = 50%
Why 70°C?
• Reasonable, realistic temperature
• White specimens rarely exceed 55°C.
• Black specimens may reach 80°C.
• These temperatures only occur near noon in
summertime.
• Produced the most realistic results – higher
temperatures were tried

Irradiance
ASTM D7869
Water Spray Step 4
1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2 Step 4
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

BP = 50°C Air = 42°C RH = 50%
Purpose: Transitional “relaxation”

from hot dry to cool wet.
• Gradually reduces thermal stresses.
• Similar temperature and irradiance as
afternoon sun gets lower.
• Unnatural cracking can occur if cold water is
sprayed on a hot specimen

Irradiance
ASTM D7869
Water Spray Step 5
1.0
0.9
0.8
0.7
0.6
Step
0.5
5
0.4
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Air = 40°C RH = 95%+
Purpose: Significant water uptake, but

less than maximum
• Maximum water uptake does not occur every day.

• Simulates days with less than maximum water
uptake.
Note: In combination with Step 6, gives a total of 180 min of wetting,
though only happens once every cycle

Irradiance
ASTM D7869
Water Spray Steps 6-9 (repeat 4x)
1.0
Steps 6-9, Repeat 4x
0.9 Cyclic Stresses (cracking)
0.8 Surface Erosion (gloss)
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Steps 6 - 9 Subcycle, Repeated 4 Times
Purpose: Rapid thermal cycling and

wet / dry cycling
• Tests mechanical and viscoelastic properties.

– Cracking & delamination
• Total time of one complete cycle is 24 hours

(first five steps + sub cycles)

Irradiance
ASTM D7869
Water Spray Step 6
1.0
0.9 Step 6
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Air = 40°C RH = 95%+
Purpose: Simulate Short Water Event
• Event such as a night with little

condensation or brief rain event.
• 30 minutes only creates water uptake in
surface layers.
• Not enough time to permeate lower layers.

Irradiance
ASTM D7869
Water Spray Step 7
1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2 Step 7
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

BP = 50°C Air = 42°C RH = 50%
Purpose: Remove water from

polymer at a controlled rate.
• Similar to Steps 2 and 4, but shorter.
• Because Step 6 was short, Step 7 can

also be short.

Irradiance
ASTM D7869
Water Spray Step 8
1.0
0.9
0.8
0.7
0.6
0.5
0.4
Step
8
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

BP = 70°C Air = 50°C RH = 50%
Purpose: Rapid heating to

create mechanical stresses
• Same conditions as Step 3, but shorter
• Time is short to promote rapid thermal cycling

– High irradiance also contributes to
photo-chemical damage
– That is a secondary purpose

Irradiance
ASTM D7869
Water Spray Step 9
1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2 Step
9
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Step 9 10 min Dark
Air = 40°C RH = 50%
Purpose: Total relaxation from all

stress
• Natural exposure has frequent periods with no

stress from sunlight, temperature or water
• A laboratory exposure with no periods of total

relaxation might cause unnatural effects, like
cracking.

Irradiance
ASTM D7869
Water Spray Reproducing Natural Weather Cycles
1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16 18 20 22 24
Time (hours)

Validating the test
method
Putting the ASTM D7869
protocol to the test

Paint Systems Tested
Automotive
• ~20 systems, multiple colors
• All systems were base coat / clear coat
• Fortified and unfortified
• Positive controls & known Florida exposure failure
mechanisms
Aerospace
• Four systems, two colors (blue and white)
• Two monocoat systems, two base coat / clear coat systems
• Florida, and in-service performance known

Potential Failure Modes to look
for in validation testing
• Chemical change
• Cracking
• Blistering
• Adhesion loss
• Color
• Gloss loss

Example: System 86
Florida Exposure SAE J2527 ASTM D7869
Expected Failure Mode: None – positive control

Observed: Excellent performance in all tests

Example: System 13
Expected Failure Mode: Slight BC/E-coat pick off.

Observed: Slight BC/E-coat pick-off on Florida and ASTM D7869

Example: System 25
Expected Failure Mode: BC/E-coat delamination.

Observed: C/E delamination on Florida pick off on New Protocol
Why such a difference?
High magnification of Panel 25
Applied coating thickness was inconsistent!

Correcting this brought FL and ASTM D7869 in line
Example: System 103
Expected Failure Mode: Blistering, gloss loss, adhesion loss

Observed: Gloss loss and adhesion loss seen on all
panels.Blistering on ASTM D7869 mimics that seen on Florida

Failure Modes
How did ASTM D7869 perform?
• Chemical change - correctly reproduced

• Cracking – correctly reproduced
• Blistering – correctly reproduced
• Adhesion loss – mostly reproduced
• Correctly reproduced after further review!
• Color - correctly reproduced

• Gloss loss – correctly reproduced

ASTM D7869 compared to SAE J2527
and Florida
• Physical failures correctly reproduced.
• Degradation chemistry is correct.
• New protocol is 40% faster

Conclusions: ASTM D7869
• ASTM D7869 accelerated lab weathering test cycle is thoroughly
researched - developed using scientific understanding of outdoor
weather phenomena – light, heat, and water
• Test cycle was validated by comparison of results to long-term

outdoor weathering data of a variety of coatings systems
• ASTM D7869 is realistic - it reproduces faithfully almost all physical

failure mechanisms and is 40% faster than current test method.
• Introduction of this new weathering protocol allows for more rapid

and accurate accelerated weathering results. These can be
correlated with outdoor test data to give powerful information.

Questions?
info@q-lab.com
www.q-lab.com

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ASTM D7869: A New Xenon-Arc

Watch Webinar Stream

Andy Francis, Q-Lab Corporation

ASTM D7869 1 We Make Testing Simple

High gloss and color integrity

Fading, cracking, peeling

Weathering testing can mean the difference between

ASTM D7869 2 We Make Testing Simple

Weathering testing can mean the difference between

ASTM D7869 3 We Make Testing Simple

Weathering testing provides crucial information

ASTM D7869 5 We Make Testing Simple

Service life prediction

ASTM D7869 6 We Make Testing Simple

Service life prediction

ASTM D7869 7 We Make Testing Simple

Service life prediction

ASTM D7869 8 We Make Testing Simple

• Not currently practical

• Shows promise for the future more for

ASTM D7869 9 We Make Testing Simple

Service life prediction

ASTM D7869 10 We Make Testing Simple

• Replicate material degradation

How can we do this?

• Hardware-based “102/18” light/light+spray standards

• SAE J2527 became the “state of the art” in 1980’s

ASTM D7869 12 We Make Testing Simple

• Standard was well-researched but did not match

• As a result, it does not adequately predict

ASTM D7869 13 We Make Testing Simple

• Outdoor weathering test dataset collected to provide

• Accelerated test cycle developed to match those real-

• Variety of materials and failure modes evaluated with

ASTM D7869 14 We Make Testing Simple

ASTM D7869 15 We Make Testing Simple

Goal: Obtain suitable body of field data to

• Weather Station Installed at

ASTM D7869 17 We Make Testing Simple

ASTM D7869 18 We Make Testing Simple

• Mass of panel measured

• Care taken to ensure no

• Able to see rain vs dew +

ASTM D7869 19 We Make Testing Simple

ASTM D7869 20 We Make Testing Simple

ASTM D7869 21 We Make Testing Simple

ASTM D7869 22 We Make Testing Simple

• 106 Combinations Prepared

• All Samples prepared by one lab

ASTM D7869 23 We Make Testing Simple

• Testing conducted per SAE J1976

• Evaluations every 6 months

ASTM D7869 24 We Make Testing Simple

ASTM D7869 25 We Make Testing Simple

• Light intensity: use higher-intensity light with

• Heat: Keep temperatures realistic, at or below

• Time of wetness: Increase! Mimic real-world

ASTM D7869 26 We Make Testing Simple

• Explored different optical filters

• Accelerated outdoor weathering

• Better match to sunlight just

ASTM D7869 27 We Make Testing Simple

ASTM D7869 28 We Make Testing Simple