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Cases from

the F-Files

Mechanisms
of Failure

Drying Curing: Topcoating Ethyl Silicate


Inorganic Zinc-Rich Primers Too Soon
By Raymond S. Tombaugh, PCS, Senior Coatings Consultant, KTA-Tator, Inc.
Richard A. Burgess, PCS, KTA-Tator, Inc., Series Editor

I
norganic zinc (IOZ) primers are one mum of 50 percent is often specified quantity is available to the resin, cure will
of the leading corrosion-inhibitive when IOZ is applied. In colder climates not be complete. (Conversely, excessive-
primers available today. They pre- humidity levels are often below 30 per- ly high humidity will inhibit evaporation of
vent corrosion so readily because cent, especially when the already dry win- solvent, leave unreacted water in the
they are highly filled with zinc powder ter air is heated in the shop. Consider porous matrix and inhibit release of the
(usually 85 percent or more by weight), that the moisture capacity of air at 40 F reaction product, ethanol.)
which serves as a sacrificial anode pre- is only about 5 grams per kilogram Similarly, shops that are located in
venting corrosion when in intimate con- (g/Kg) of air. A relative humidity of 40 the arid west and southwest can also
tact with well-prepared steel. percent contains only about 2 g/Kg. This encounter curing issues as a result of
However, the inorganic zinc primers same quantity of moisture is equivalent dry air. It is not uncommon to see rela-
come with their own set of limitations. to 20 percent relative humidity at about tive humidity conditions in the 10 to 20
Specifically, problems can arise with 60 F. IOZ requires a finite amount of percent range in Nevada, Arizona and
adequate curing prior to overcoating. water to properly cure and until that the surrounding states. While some
IOZs cure uses the following reaction: shops may have
humidity-controlled
Si (OC2H5)4+ 4H2O atmospheres, limit-
SiO compounds + C2H6O ed interior storage
space will often
Essentially, tetraethyl orthosilicate lead to moving par-
[Si(OC2H5)4] and other alkyl silicates tially cured primed
react with airborne moisture/water, components out-
releasing ethanol. A silicate-based doors where
structure is formed. Problems arise humidity may be
when there is insufficient moisture pre- low. These dry con-
sent in the air to ensure a complete ditions will cause
reaction of the silicates. solvents to evapo-
While some manufacturers require a rate rapidly from
Fig. 1: Pictured here is a bridge where only one girder had thick, uncured zinc.
minimum relative humidity of 40 percent Note the significant failures. The other girders were cured and had no failures. the film, resulting
in order to ensure adequate cure, a mini- Photos courtesy of KTA-Tator, Inc. in a dry but

paintsquare.com / JPCL September 2014 17


F-Files: Mechanisms of Failure

uncured primer. If the applicator knows coated too soon, the product is essen- ture long enough to fully cure. That is,
that IOZ primers react with moisture to tially sealed off from the available mois- IOZ primers are not traditionally consid-
cure and recognizes that arid condi- ture and a complete cure may never be ered a rapid recoat product, especially
tions exist, the primed surfaces can be achieved. In steel fabrication and in under dry conditions. This is counterin-
misted with water an hour or so after blast and paint shops, production rates tuitive for some.
application in order to facilitate the cur- are always a concern and multiple coat The curing of inorganic zinc primers
ing reaction. Multiple applications of systems can present a bottleneck. In may also be inhibited by the application
water may be necessary, because the the past, only the primer coat was of thicker film builds. Traditionally, the
water will also evaporate from the sur- applied and the IOZ had more than standard thickness has been 2 to 3
faces rapidly under arid conditions. ample time to cure during shipping and mils dry film thickness (DFT). In more
Special fans equipped with water atom- storage. Today, two- or three-coat sys- recent years some manufacturers have
izers can also be effective. Misting the tems may all be applied in the shop in increased the recommended thickness
primed surfaces with water or saturat- order to limit the amount of field paint- up to 6 or 7 mils, perhaps to avoid
ing the floor with water to increase the ing required. Limited shop floor area rejection of excess thickness in overlap
relative humidity in the shop must be often dictates that the steel be fabricat- areas such as web or flange interfaces.
done reasonably soon after application ed, abrasive blast cleaned, primed and When overly thick IOZ films are
(i.e., within one to two hours), as the overcoated with one or more finish applied, moisture may have a more diffi-
reaction with moisture must occur early coats in rapid succession to improve cult time penetrating through the cross-
in the curing phase. shop throughput. When this occurs, the section and curing the film. Although
When uncured IOZ primers are over- primer may not be subjected to mois- often thought to be self-policing via
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18 JPCL September 2014 / paintsquare.com


the presence of micro-cracking or mud- relative resistance rating is assigned
cracking when applied excessively thick, based on the double-rub test. A rating
that is not always the case. Micro-crack- of 5 indicates that there was no effect
ing may never be discovered until a on the surface, while a rating of 0 indi-
coating failure occurs. cates that the film was penetrated to
Inorganic zinc primers can be the substrate in 50 double rubs or less.
assessed for degree of cure using two Note that a small amount of discol-
relatively simple tests. The first test, oration may be present on the cloth
described in ASTM D4752, Standard (due to burnishing of the zinc) even
Practice for Measuring MEK Resistance though the primer is cured. The specifi-
Fig. 2: This photo shows an area where the IOZ
of Ethyl Silicate (Inorganic) Zinc-Rich er may invoke a minimum resistance had been exposed for a couple weeks. When the
Primers by Solvent Rub, involves rub- rating based on the ASTM standard topcoats were pulled away separation occurred
within the zinc layer, with zinc on the back of the
bing the surface of the primer back and prior to over coating the IOZ. delamination and left on the bridge.
forth (double rub) for fifty times with a The second test, the coin rub test,
white cloth saturated in methyl ethyl has no industry standard to describe it. primer will burnish (become shiny),
ketone (MEK). The binder in the However, it is widely used to assess while an uncured primer will powder.
uncured film is soluble in MEK and can cure and is fairly reliable. It is conduct- While impractical in the shop or field,
be removed if it is not completely ed by rubbing the edge of a coin (for the cure rate of inorganic zinc primers
cured; while a completely cured film is example a nickel) across the surface of can be monitored using laboratory ana-
not soluble and will resist the solvent. A the primer. The surface of a cured IOZ lytical techniques including Fourier

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paintsquare.com / JPCL September 2014 19


F-Files: Mechanisms of Failure

Transform Infrared Spectroscopy. ing the weakened primer to cohesively


Samples can be prepared and spectra separate. Epoxy mid-coats are often
obtained at various time intervals and the next coat that is applied after the
under varying curing conditions of tem- primer. These coatings contain strong
perature and humidity. The cure ratio solvents that penetrate the uncured
can be determined based upon the dis- primer and the epoxy resin exerts
appearance of organic groups by inte- stress on the underlying layer during
gration of the areas of absorption spec- the crosslinking process. Naturally, an
tral bands due to the aliphatic carbon- increased thickness in the zinc primer
hydrogen stretching vibration near Fig. 3: Excessive impact damage on a light rail or overcoats worsens the problem.
line that occurred during erection is visible in this
2900cm-1 relative to the silicate vibra- image. A recent Cases from the F-Files col-
tions near 1050cm-1. umn (Can In-Process Quality Control
Visual evidence of coating system fail- mil or two of zinc remains behind but in Prevent Premature Coating Failure?
ure due to over coating uncured inor- a relatively short time period (a few JPCL, January 2013) described several
ganic zinc may be immediate or may be weeks), the uncured zinc is worn away case studies of coating failures that
delayed. If years pass by prior to notic- and rust appears on the surface of the were caused in part by a lack of quality
ing the problem, the failure may steel. control. Case Study No. 3 is repeated
become catastrophic including wide- The delamination typically occurs due on the next page because it clearly
spread delamination cohesively within to the stresses imparted by the coating illustrates the phenomena described in
the inorganic zinc primer. Generally, a layer(s) applied over the primer, caus- this column.
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20 JPCL September 2014 / paintsquare.com


no more moisture could react with and the contractive curing stresses
Case Study No. 3: You Know
the primer, since it was effectively imparted by the epoxy caused the
What They Say, Dry Heat is
sealed off by the epoxy. The zinc zinc primer to cohesively split.
More Comfortable
primer remained in a dry, but Since the web and flange are adja-
Background:
uncured (and weakened state). The cent to one another, the thickness
The project specification required
solvents from the epoxy mid-coat of the epoxy was slightly higher
abrasive blast cleaning to achieve a
penetrated the uncured primer, along the fillet weld area. The
Near-White Metal finish per SSPC-
SP 10/NACE No. 2 and the applica-
tion of an inorganic zinc primer to
structural steel components in the
fabrication shop. Application of the
intermediate coat was also per-
formed in the shop, while the top-
coat was scheduled for application
in the field after erection and bolt-
ing of the steel. The work was done
in the winter months and the shop
was heated. The fabricators quality
control specialist kept documenta-
tion revealing that they had con-
formed to the thickness and recoat
times recommended by the coating
manufacturers technical representa-
tive, who visited the shop during
coating application activities. The
steel was loaded onto trucks and
shipped to the site. Upon arrival at
the construction site spontaneous
cracking of the coating along the fil-
let weld (where the web and flange
are joined) was discovered. That
cracking and lifting along the fillet,
and the poor adhesion of the coat-
ing system on the web was evident.
Examination of a disbonded coating
chip revealed the presence of zinc
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primer on the back side of the chip


and on the steel surface, indicating
that the location of break was cohe-
sive within the zinc primer.
Cause:
Ethyl silicate type inorganic zinc-
rich primers require moisture to
cure. In this case, an insufficient
length of time was allowed before
the application of the epoxy mid-
coat. Once the epoxy was applied,

paintsquare.com / JPCL September 2014 21


F-Files: Mechanisms of Failure

higher thickness exacerbated the Avoidance Through Quality within the prevailing environment.
problem and resulted in the crack- Control Inspection? The key is to verify that the condi-
ing and detachment. When other Inorganic zinc-rich primers dry tions of temperature and humidity
areas were evaluated, it became very quickly (especially in a heated (listed on the product data sheets)
evident that the entire system was environment); however they may are present in the shop prior to
at risk for failure. not cure for many hours or even application and to verify that the
days if the humidity is too low cure has been achieved, rather
than relying on cure-time tables
provided by the coating manufac-
turer, or assuming that drying and
curing are synonymous. Quality
control inspection by the fabricator
should have included a curing test.
In fact there is one specifically
designed for the type of coating
described by this case study
(ASTM D4752, referenced earlier).
Once a resistance rating of 4 or 5
is achieved (after 50 double rubs)
the zinc-rich primer can be consid-
ered cured and ready for recoat-
ing. Some manufacturers rely on
pencil hardness data instead of
solvent resistance to assess cure.
Either way, a knowledgeable QC
inspector knows how specific coat-
ing types cure, the conditions that
are necessary for the reactions to
occur, and the tests that are avail-
able to verify coating film proper-
ties prior to overcoating.

While it may take some time for the


failure to reveal itself, some telltale
signs are often evident during the stor-
age and erection processes. These
observations may be disregarded as
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normal coating defects by construction


companies or coating manufacturers.
One indication that there is a problem is
when there is an excessive amount of
impact damage that occurs during erec-
tion. The topcoats are exerting stresses
on the weakened IOZ primer. When the
coating is impacted, the stress is
relieved and the coating literally pops
off of the surface, typically separating

22 JPCL September 2014 / paintsquare.com


cohesively within the zinc primer layer. About the Author preparation, project management and
This problem can be exacerbated by Ray Tombaugh is a other coatings-related services. He
the application of thick topcoats as senior coatings con- holds a B.S. in chemical engineering
even greater stresses are exerted on sultant for KTA-Tator, from Lehigh University, is an SSPC-cer-
the primer. Inc., providing coat- tified Protective Coatings Specialist and
A second indicator of a problem is ings failure analysis, a NACE-certified Coating Inspector
when large delaminations occur after condition assess- Level 3 (Peer Review).
one or two winters. The stresses ment, specification JPCL
caused by thermal expansion and con-
traction of the steel members may
cause spontaneous delaminations.
These failures may be isolated to only a
few areas but are indications that the
problem may be more widespread. Of
course, the wearing away of the
remaining IOZ film after it is exposed
and the formation of rust on the sur-
face of the steel is another indicator of
a problem.

Conclusions
In summary, the key parameters in
assuring a sound application of inorganic
zinc are to:
1. Apply the primer at the correct thick-
ness;
2. Verify that the primed steel is stored
in an area with relative humidity condi-
tions above the coating manufacturers
minimum and ideally in excess of 50
percent;
3. Verify that the primer is allowed to
cure for the manufacturers recom-
mended cure time under conditions of
temperature and humidity; and
4. Verify the cure using the solvent rub
test or other prescribed procedures.
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Never assume the zinc primer has


cured just because the prevailing condi-
tions conformed to the manufacturers
product data sheets. Cure times may
need to be adjusted if the primed com-
ponents are stored at locations with
varying ambient conditions.

paintsquare.com / JPCL September 2014 23


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