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coatings

Review
Intumescent Coatings for Fire Resistance of Steel Structures:
Current Approaches for Qualification and Design
Donatella de Silva 1, *, Iolanda Nuzzo 2 , Emidio Nigro 1 and Antonio Occhiuzzi 2

1 Department of Structures for Engineering and Architecture, University of Naples Federico II,
80138 Napoli, Italy; emidio.nigro@unina.it
2 Construction Technologies Institute, National Research Council of Italy, Polo Tecnologico di San Giovanni
a Teduccio, 80146 Napoli, Italy; nuzzo@itc.cnr.it (I.N.); occhiuzzi@itc.cnr.it (A.O.)
* Correspondence: donatella.desilva@unina.it

Abstract: Intumescent coatings (ICs) are often used for protecting steel buildings during a fire when
the structural, aesthetic, and architectural features of the structural members should be preserved.
Indeed, ICs form a thin protective layer on the steel surface, that if exposed to fire or elevated
temperatures, expands in volume with a consequent reduction in density. Hence, the protective
layer captivates heat and protects the structural member from damage or elevated deformation. This
reactive fire protection is designed using prescriptive tables, in which the IC thickness is chosen
according to the required fire resistance, critical temperature, and section factor of the steel element.
These tables are elaborated on the basis of the tests results according to the UNI EN 13381-8 standard,
which is the reference for characterizing reactive systems such as ICs. For its reactive nature, this fire
protection has to be applied to the structure in a controlled manner, and it is good practice to verify
its correct application by measuring thickness and adhesion in situ through regulated methods. The
qualification process of IC systems in Italy can be realized through a voluntary certification within the
scope of a European technical assessment or by means of a national technical assessment certificate
that is mandatory. All these aspects related to qualification, assessment, and design of ICs are often
Citation: de Silva, D.; Nuzzo, I.;
ignored by both designers and manufacturers, especially in Italy. Therefore, this paper describes all
Nigro, E.; Occhiuzzi, A. Intumescent
the approaches, introducing the main technical differences, in order to provide a sort of guideline on
Coatings for Fire Resistance of Steel
the use of these reactive fire protections.
Structures: Current Approaches for
Qualification and Design. Coatings
2022, 12, 696. https://doi.org/
Keywords: fire resistance; certification; intumescent coating; steel structures
10.3390/coatings12050696

Academic Editor: Ivan Jerman

Received: 19 April 2022 1. Introduction


Accepted: 17 May 2022 In the current Italian regulatory framework, when a steel structure is designed, a given
Published: 19 May 2022 fire resistance is often required, but generally due to the low fire performance of steel,
Publisher’s Note: MDPI stays neutral
this requirement cannot be satisfied. An increase in the fire resistance duration for steel
with regard to jurisdictional claims in structures can be reached by applying fire protection materials, preventing the achievement
published maps and institutional affil- of high temperatures in steel members during fire [1]. These protection materials can be
iations. divided into two categories: passive materials (e.g., incombustible boards) and reactive
materials (e.g., intumescent coatings). Intumescent coating (IC) is reactive because it swells
as a result of heat exposure, increasing many times its original thickness and decreasing in
density, producing a carbonaceous char formed by a large number of small bubbles that act
Copyright: © 2022 by the authors. as an insulating layer to protect the substrate.
Licensee MDPI, Basel, Switzerland. The advantages of this protection system include reduced invasiveness compared to
This article is an open access article other materials, an easy application, and a good surface finishing. Indeed, the rapid growth
distributed under the terms and in the use of ICs in the built environment is associated with the low impact in the attractive
conditions of the Creative Commons
architectural appearance of bare steel structures, along with their light weight and their
Attribution (CC BY) license (https://
flexibility for both on- and off-site applications [2]. Thin film intumescent coatings (ICs)
creativecommons.org/licenses/by/
are solvent- or water-based systems applied with a dry thickness ranging between 400 and
4.0/).

Coatings 2022, 12, 696. https://doi.org/10.3390/coatings12050696 https://www.mdpi.com/journal/coatings


Coatings 2022, 12, 696 2 of 17

3000 µm, and they are typically used for general construction including structural steel
with an ISO834 fire curve. In contrast, thick film coatings tend to find use in the oil and
gas industry, such as for protecting petroleum refineries, considering the hydrocarbon fire
curve [3]. These ICs can be used not only for fire protection of steel but also for wood or
concrete structures. In the case of wood, novel methods for calcium carbonate deposition
in wood that increases carbon dioxide concentration and fire resistance are also proposed
in the literature [4]. For concrete, especially if a geopolymer one is considered, several
coating types can be considered in order to increase its fire resistance [5]. While, for steel, IC
remains one of the best ways to prevent high temperatures in the structures, during fires.
According to the Italian design code NTC2018 [6], all materials and products employed
for structural use shall comply with a qualification process that can be pursued according
to three alternative cases.
In case A, the performance assessment of the material/product is regulated by a
specific harmonized European standard (hEN) published in the Official Journal of European
Union (OJEU). Manufacturers are obliged to mark CE on their products if covered by hENs
and to report the relative essential characteristics in the Declaration of Performance (DoP),
according to the European construction product regulation (CPR) no. 305/2011 [7]. In case
B, due to the absence of such harmonized regulations, the qualification process is controlled
by the NTC2018 code itself. This is, for instance, the case of reinforced concrete. Finally,
case C refers to all materials and products not belonging to cases A or B, comprehending
the most innovative and new solutions.
In this case, the manufacturer shall achieve the CE labeling of the product on the
basis of a European Technical Assessment (ETA) or shall obtain a technical assessment
certificate. The ETA can be released by a specific body called TAB (i.e., Technical Assessment
Body), designated by a Member State and part of the European Organization of Technical
Assessment (EOTA). The ETA is a document providing the product performances assessed
according to methods and criteria described in a European Assessment Document (EAD),
that is a specific product standard. Once the ETA is released, the manufacturer can produce
the Declaration of Performance and obtain a voluntary certification that allows the free
trade of the product on the European market.
Alternatively, the manufacturer of a product belonging to case C can opt for obtaining
a national technical assessment certificate, released by the President of the Superior Council
of Public Works on the basis of guidelines produced by the Central Technical Service,
eventually in agreement with the National Fire and Rescue Service for those products
requiring the assessment of the resistance to fire.
Performance of the assessment of IC systems is not covered by any harmonized
standard, and there are no indications in the NTC2018 design code. Thus, the qualification
process of such product complies with case C described above. In order to obtain a national
technical assessment certificate concerning the IC resistance to fire, EN 13381-8:2013 [8]
shall be exclusively adopted for reactive materials according to indications by the National
Fire and Rescue Service [9].
On the basis of test results according to EN 13381-8:2013, it is possible to relate the
fire resistance period, section factor, and the thickness of the fire protection material to
maintain the steel’s temperature below the design temperature. These data are input
into the design process of ICs for the protection of steel structures. Alternatively, the
manufacturer can undertake a voluntary certification process with a TAB in order to get an
ETA on the basis of EAD 350402-00-1106 [10], which comes from the conversion of ETAG
018 part 2 [11], and specifically concerns the performance assessment of reactive coatings
for fire protection of steel elements. However, there is still a lack of a harmonized reference
that provide manufacturers, designers, and contractors with recommendations for testing,
design, installation, and control.
The aim of the paper was to give an overview of the various approaches in terms
of assessment and certification of the IC and to design the fire resistance of protected
steel structures, highlighting the various aspects that characterize national and European
The aim of the paper was to give an overview of the various approaches in terms of
Coatings 2022, 12, x FOR PEER REVIEW
assessmentand certification of the IC and to design the fire resistance of protected 3 of 18 steel
structures, highlighting the various aspects that characterize national and European pro-
Coatings 2022, 12, 696 3 of 17
cedures, after introducing a technical description of the IC system and its functioning.
The the
Indeed, aimcomplicated
of the paper was to give and
industrial an overview of the various
low requirements for approaches in terms
the use of these of
products for
assessment and certification of the IC and to design the fire resistance of protected
the fire-protected steels in practice is commonly not well known. Thus, the work is in- steel
structures, highlighting the various aspects that characterizeof national and European
procedures, after introducing
tended as a guidance concerninga technical description
certification procedures therequired
IC system and its
in Italy inpro-
functioning.
relation to
cedures, after introducing a technical description of the IC system and its functioning.
Indeed, the complicated
the EU norms industrial
and regulations. and low
A general requirements
outlook for the
of the required useand
tests of these products
procedures is
Indeed, the complicated industrial and low requirements for the use of these products for
for the fire-protected steels in practice is commonly not well known. Thus, the work is
presented.
the fire-protected steels in practice is commonly not well known. Thus, the work is in-
intended
tended as aasguidance
a guidance concerning
concerning certification
certification procedures
procedures required required
in Italy in in Italy to
relation in relation
2.
to IC
the Technical
EU norms Solution
and regulations. A general outlook of the required
the EU norms and regulations. A general outlook of the required tests and procedures is tests and procedures
is presented.
ICs are always part of a system including an anticorrosive primer and, generally, a
presented.
topcoat are used for steel structures. The primer ensures adhesion to the substrate in the
2.
2. ICTechnical
IC TechnicalSolution
Solution
normal state, anticorrosion protection, and stickability of the intumescent char formed
during ICsfire
ICs areexposure,
are always
always part
part of of
while a system
a system
the including
including
topcoat has an an anticorrosive
anticorrosive
both aesthetic primer primer
and,
function, itand,
andgenerally, generally,
is useda to pro- a
topcoat
topcoat are
are used
used for
for steel
steel structures.
structures. The The
primerprimer ensures
ensures
mote weathering resistance in end-use conditions (see Figure 1). adhesion
adhesion to the to the
substrate substrate
in the in the
normal state,
normal state,anticorrosion
anticorrosion protection, and and
protection, stickability of the of
stickability intumescent char formed
the intumescent char formed
during fire
during fireexposure,
exposure,while
whilethethetopcoat
topcoathas both
has aesthetic
both function,
aesthetic and and
function, it is used to pro-
it is used to promote
mote weathering
weathering resistance
resistance in end-use
in end-use conditions(see
conditions (seeFigure
Figure 1).
1).

Figure 1. Intumescent system.


Figure 1. Intumescent system.
FigureAs
1. Intumescent system.
also described before, this reactive protection, by swelling and forming a large
number of small bubbles, acts as
As also described before, this an insulating layer, with very
reactive protection, small thermal
by swelling conductivity,
and forming a large
As also described before, this reactive protection, by swelling and forming a large
to protect
number ofthe steel
small substrate
bubbles, from
acts as antheinsulating
high temperatures
layer, withgenerated
very smallbythermal
the fire conductivity,
(see Figure
number of small bubbles, acts as an insulating layer, with very small thermal conductivity,
2).protect
to
to protectthe
thesteel
steelsubstrate
substrate from
from thethe high
high temperatures
temperatures generated
generated by theby the
fire fireFigure
(see (see Figure 2).
2).

Figure
Figure2.2.Fire
Firebehavior
behaviorof of
ICs.
ICs.
Figure 2. Fire behavior of ICs.
The
Thebehavior
behavior of ICs subjected to elevated temperatures has been largelylargely
investigated
The behavior ofof ICs
ICs subjected
subjectedto toelevated
elevatedtemperatures
temperatureshas hasbeen
been largelyinvestigated
investigated
in recent
in recent studies,
recent studies, especially
studies, especially from
fromthe chemical
the point
chemical of
pointview. It is
ofofview. well known
ItItisiswell that thethat the
known
in especially from the chemical point view.
intumescent process is a complex chemistry including the organic (coating) binder resin
well known that the
intumescent
intumescent process
process is a complex
is athe
complex chemistry
chemistry including
including the organic
the organic (coating)
(coating) binder
binder resin
resin
and an acid catalyst like ammonium polyphosphate, which decomposes to yield a
and an
and an acid
acid catalyst
catalyst like
like the
the ammonium
ammonium polyphosphate,
polyphosphate,which
whichdecomposes
decomposestotoyield
yielda a
mineral acid. This acid reacts with a carbonific source, such as pentaerythritol, to produce
a carbon char. The melanine, which is a foam-producing agent, reacts with the acid source
and decays, changing into an inert gas that then expands the char. This is the description
of the main reactions that basically take place, although more complex interactions occur
too. For example, filler particles are incorporated into the formulation to act as nucleating
sites or “bubble growth” locations and the resin binder theatres a large part in softening
and charring [12]. This chemical transformation affects the thermal properties of ICs [13].
mineral acid. This acid reacts with a carbonific source, such as pentaerythritol, to produce
a carbon char. The melanine, which is a foam-producing agent, reacts with the acid source
and decays, changing into an inert gas that then expands the char. This is the description
of the main reactions that basically take place, although more complex interactions occur
Coatings 2022, 12, 696 too. For example, filler particles are incorporated into the formulation to act as nucleating 4 of 17

sites or “bubble growth” locations and the resin binder theatres a large part in softening
and charring [12]. This chemical transformation affects the thermal properties of ICs [13].
Andersen [14]
Andersen [14] proposed
proposed the
the development
developmentofofthermal
thermalresistance
resistanceover
over time
timedivided
divided intointo
four general
four general phases, which
which were
werealso
alsoconfirmed
confirmedandandidentified byby
identified dede Silva et et
Silva al. al.
in [15],
in [15],
investigating the
investigating the thermal conductivity
conductivityand andswelling
swellingofofICs
ICs(Figure
(Figure3).3).

35 ΔdIC(mm) 0.25
λIC(W/mK)

End of swelling
30 1- Inert
reaction
phase
0.2
dIC
25
2-Transient
phase 0.15
20

15 3- Steady phase 0.1

10
Activation
point 0.05
5 λIC
Minimum of λIC

θ (°C)
0 0
0 100 200 300 400 500 600 700
Figure3.3. Common
Figure Common trends
trends in
in the
the thermal
thermalequivalent
equivalentconductivity
conductivityand ICIC
and swelling and
swelling definition
and of of
definition
the four general phases in their development.
the four general phases in their development.

The phases
The phases of
of IC
IC behavior
behaviorreported
reportedininFigure
Figure3 3arearebriefly
briefly described
described in in
thethe
following.
following.
1. 1. Inert phase
Inert phase
Before
Before reaching its reaction
reaching its reaction temperature,
temperature,the thedry
dryICICisisinert
inert
toto the
the temperature
temperature andand
the
the thickness is equal to the initial one. During this phase, the IC is gradually melting andand
thickness is equal to the initial one. During this phase, the IC is gradually melting
increasing
increasingits
itsviscosity
viscositysignificantly.
significantly.The
Thethermal
thermal resistance
resistance provided
provided to to the
the steel
steel is
is minimal
mini-
and
malthe
andmeasured protected
the measured temperature
protected is similar
temperature to the
is similar unprotected
to the unprotected one. one.
2. 2. Transient
Transient phase
phase
During the transient phase, the IC starts to swell and quickly increases in volume.
During the transient phase, the IC starts to swell and quickly increases in volume.
When all the virgin material is consumed and the blowing agent is exhausted, a multicellular
When all the virgin material is consumed and the blowing agent is exhausted, a multicel-
black char structure forms the IC. Generally, at this moment, the minimum thermal IC
lular black char structure forms the IC. Generally, at this moment, the minimum thermal
conductivity within the transient phase and the intumescent char is considered fully
IC conductivity within the transient phase and the intumescent char is considered fully
developed (see Figure 3). Furthermore, at this point, the char assembly is characterized by
developed (see Figure 3). Furthermore, at this point, the char assembly is characterized by
a black color due to the high carbon binder quantity. Later, the increase in the thermal IC’s
a black color due to the high carbon binder quantity. Later, the increase in the thermal IC’s
conductivity is related to the gradual consumption of the carbon binder, which is the main
conductivity is related to the gradual consumption of the carbon binder, which is the main
component creating the char structure.
component creating the char structure.
3. Steady phase
3. Steady phase
The endothermic reaction finishes when all the combustible materials burned and
the IC pass in the steady phase. At this stage, only the white expanded char structure
contributes to the thermal conductivity, keeping it to a constant value or sometimes it
slightly increases.
4. Post-austenitization phase
For temperatures greater than 700 ◦ C, after reaching the austenitization point, the IC
char structure looks like a fragile and inconsistent material, characterized by a light white
color. At this point, the carbon binder is all burned, and with that the char structure is
degraded, losing its cohesion. During the post-austenitization phase and at high tempera-
tures, the char structure starts to crack. The thermal IC conductivity increases by a steady
value with a consequent increment in the steel temperature. The cracks act as thermal
channels, and the char structure stops providing good insulation to the steel surface.
Coatings 2022, 12, 696 5 of 17

3. Qualification Process
The qualification process of ICs in Italy can follow a national or a European approach.
In the first case, fire resistance shall be tested according to UNI EN 13381-8 [8], which
contains a series of fire tests on steel elements protected with the IC that has to be qualified.
In order to ensure free trade in the European market, the qualification process is regulated
by EAD 350402-00-1106 [10] in the context of voluntary certification. Key points of both
procedures are addressed in the following section in order to provide an overview of the
main differences.

3.1. National Qualification Process


The UNI EN 13381-8 specifies a test method for determining the contribution of
applied fire protection systems to structural steel members. This evaluation was designed
to cover a range of thicknesses of ICs, a range of steel sections characterized by their section
factors Am /V (which is the ration between the element surface exposed to fire Am and
its total volume V), a range of design temperatures, and a range of valid fire protection
classification periods. In particular, several steel elements have to be tested: unloaded
tall columns and short columns, unloaded and loaded beams, and varying the section
factors and the IC thickness. Generally, the beams are mounted to the ceiling of the furnace
and the ends of the beams are protected in accordance with EN 13381-8:2013, and these
beams are heated from three sides. The standard furnace is generally 4 m long and 3 m
wide, equipped with several burners and controlled by a programmable logic controller to
simulate different fire curves. Figure 4 shows an example of an arrangement in a 6furnace
Coatings 2022, 12, x FOR PEER REVIEW of 18 of
fire tests conducted according to EN 13381-8:2013, in which the IC thickness varies between
1500 and 2500 µm.

Figure 4. Typical disposition of specimens for a fire test according to EN 13381-8.

FigureThis
4. Typical disposition
European of specimens
Standard for the
contains a firefire
testtest
according to EN 13381-8.
procedures that specify the tests that
should be carried out to determine the efficiency of the fire protection system to remain
1200 θ θ[°C]
(°C)

1000
Coatings 2022, 12, 696 6 of 17

attached to the steelwork and to provide data on the thermal properties of the fire protection
system when exposed to the standard temperature/time curve specified in EN 1363-1 [16].
In some cases, the code require tests in furnaces under a slow heating curve in order to
evaluate whether the performances of the ICs are affected by fire curves (Figure 5) with
low thermal gradients (e.g., smoldering fire) [17]. If the ICs are used to protect structures in
which the potential fire is similar to a hydrocarbon one, the standard curve appropriate to
Figure 4. Typical disposition of specimens for a fire test according to EN 13381-8.
this fire has to be used.

1200 θ θ[°C]
(°C)

1000

800

600

400 Hydrocarbon fire curve


ISO 834 fire curve
Smouldering fire curve
200

tt [min]
(min)
0
0 15 30 45 60 75 90 105 120
Figure 5.
Figure 5. Fire
Fire curves.
curves.

In addition, current methods for testing and approving ICs for commercial use impli-
cate the coating in a full-scale beam and column using a standard process in a furnace. This
procedure must be repeated, even if the manufacturer has only made a minor change to the
chemical formulation.
The fire test methodology makes provisions for the collection of data, which can be
used as direct input into the calculation of the fire resistance of the steel structural members
in accordance with the procedures given in EN 1993-1-2 [18] and EN 1994-1-2 [19]. This
European Standard also contains the assessment, which prescribes how the analysis of the
test data should be made and gives guidance on the procedures by which interpolation
should be undertaken.
The assessment is performed in two main steps: first is the physical presentation,
which is generally determined by evaluating the difference in temperature data between
loaded and unloaded elements and checking if there is a negative influence from the
application of a load. From this assessment, a temperature-dependent correction factor is
calculated, which is applied to all the unloaded columns involved in the test set. These
unloaded columns are in accordance with the standard tests included in the thermal
performance evaluation.
The results of these tests and the assessment obtained according to this standard are
directly applicable to steel sections of I and H cross-sectional shapes and hollow sections
(see Figure 6).
plication of a load. From this assessment, a temperature-dependent correction factor is
calculated, which is applied to all the unloaded columns involved in the test set. These
unloaded columns are in accordance with the standard tests included in the thermal per-
formance evaluation.
The results of these tests and the assessment obtained according to this standard are
Coatings 2022, 12, 696 7 of 17
directly applicable to steel sections of I and H cross-sectional shapes and hollow sections
(see Figure 6).

1200 θ (°C)
1100

1000

900

800

700

600

500

400

300 ISO834
IPE200_1275 µm
200
D219.1xT8_2500 µm
100 HE400M_1237 µm
t (min)
0
0 20 40 60 80 100 120
Figure 6.
Figure 6. Specimens’
Specimens’ temperatures
temperatures measured
measured during
duringthe
thefire
firetest.
test.

The second
The second step
step isisthe
theelaboration
elaborationof ofthe
thetesttestdata
datafor
forthe
thedrafting
draftingofofprescriptive
prescriptivetables
ta-
bles useful for the design of the IC thickness as a function of required fire resistance,
useful for the design of the IC thickness as a function of required fire resistance, critical crit-
ical temperature,
temperature, and and
sectionsection factor
factor of steel
of the the steel element
element (see(see
TableTable 1). The
1). The critical
critical temper-
temperature
ature ranges between 500 and ◦ 600 °C and is the one at which the steel
ranges between 500 and 600 C and is the one at which the steel element loses its load- element loses its
load-bearing
bearing capacity
capacity at a specific
at a specific load;load; the higher
the higher the critical
the critical temperature,
temperature, thethe lower
lower thethe
fire
fire protection
protection required
required by theby structure.
the structure.

Table 1. Typical table for the prescriptive design of IC thickness.

Fire Resistance Classification


Critical temperature (◦ C) 350 400 450 500 550 600 650
Section factor A/V (m−1 ) Thickness of IC (µm)
70 600 400 400 400 400 400 400

75 600 400 400 400 400 400 400

80 600 400 400 400 400 400 400

85 600 400 400 400 400 400 400

90 600 400 400 400 400 400 400

95 750 400 400 400 400 400 400

100 750 400 400 400 400 400 400

105 750 400 400 400 400 400 400

This assessment prescriptive method treats ICs as chemically nonreactive materi-


als, and it implicitly assumes that thermal properties only depend on the temperature,
representing, in some cases, a limitation of IC use in design and verification methods.
Coatings 2022, 12, 696 8 of 17

3.2. European Qualification Process


The European qualification of reactive coating for fire protection of steel elements is
regulated by the EAD 350402-00-1106 [10], published in the OJEU in 2017. This standard
covers the reacting coating only or the reactive coating kit, composed of the primer for
corrosion protection or as a bonding agent, the reactive component, and the topcoat (see
Figure 1). The assessment methods included in the EAD refers to the fire protective
coating element/kit with an intended working life from a minimum of 10 years up to
25 years. The product performances can be expressed through the assessment of the
essential characteristics provided in Table 2.

Table 2. Essential characteristics and relative assessment methods for reactive coating systems
according to EAD 350402-00-1106.

Essential
No. Assessment Method
Characteristic
Basic Work Requirement 2: Safety in case of fire
1 Reaction to fire Test methods and classification according to EN 13501-1 [20]
2 Resistance to fire Test methods and classification according to EN 13501-2 [21]
Basic Work Requirement 3: Hygiene, health, and the environment
Content, emission, and/or release
3 SVOCs and VOCs according to EN 16516
of dangerous substances
Basic Work Requirement 4: Safety and accessibility in use
4 Adhesion Insulating efficiency tests according to EN 1363-1
5 Durability Insulating efficiency tests on initial and exposed specimens according to EN 1363-1

Reaction to fire tests can be performed according to EN 13823 [22] or EN 11925-2 [23],
applying the largest possible quantity of reactive fire protection on a steel surface with a
thickness of at least 2 mm. The result of the tests applies to all reactive coating systems with
application quantities smaller than or equal to the application quantity tested according
to [22], including all primers and topcoats.
Fire resistance is assessed by means of the test method described in EN 13381-8 [5].
Because a reactive coating system does not possess fire resistance on its own, the classifica-
tion applies to the protected element, including the reactive coating system, and not to the
protection itself.
The performance of the product in terms of content, emission, and/or release of
dangerous substances needs to be assessed on the basis of the intended release scenario
that can be:
• IA1: Product with direct contact to indoor air;
• IA2: Product with indirect contact to indoor air but possible impact on indoor air;
• S/W2: Product with indirect contact soil, ground, and surface water.
Semi-volatile organic compounds (SVOCs) and volatile organic compounds (VOCs)
should be determined in accordance with EN 16516 [24].
The durability of the fire protective coating system is assessed with respect to service
conditions, such as humidity, variations in temperature and relative humidity, rain and
radiation of the sun, and chemical attacks. The durability assessment is achieved by means
of indirect testing, i.e., through the measurement and comparison of insulating efficiency
in initial (virgin) and exposed (to several conditioning) specimens. Insulating efficiency
tests are performed according to a small-scale furnace fire test under the conditions of the
standard time–temperature curve as defined in EN 1363-1 [16]. Specimens can be panels or
I-section short columns. Fire tests finish when the specimen’s mean temperature reaches
500 ◦ C. When the mean time to achieve the critical steel temperature t500 on exposed
specimens is not less than 85% of the time t500 registered on virgin specimens, the durability
is deemed to be met.
in initial (virgin) and exposed (to several conditioning) specimens. Insulating efficiency
tests are performed according to a small-scale furnace fire test under the conditions of the
standard time–temperature curve as defined in EN 1363-1 [16]. Specimens can be panels
or I-section short columns. Fire tests finish when the specimen’s mean temperature
Coatings 2022, 12, 696
reaches 500 °C. When the mean time to achieve the critical steel temperature t500 on ex-
9 of 17
posed specimens is not less than 85% of the time t500 registered on virgin specimens, the
durability is deemed to be met.
In order to ensure the required fire protective performance, adhesion of the reactive
In order to ensure the required fire protective performance, adhesion of the reactive
coating system to its substrate is fundamental. Adhesion is covered by testing the insulat-
coating system to its substrate is fundamental. Adhesion is covered by testing the insulating
ing efficiency as previously introduced.
efficiency as previously introduced.
4.
4. Design
Design and
and Control
Control ofof the
the Application:
Application: Overview
Overview of of Available Codes
Available Codes
4.1.
4.1. Design
Design and
and Verification Methods with
Verification Methods with aa Prescriptive-Based
Prescriptive-Based Approach
Approach
According
According to
to current
current regulations,
regulations, the
the fire
fire resistance of steel
resistance of steel structures
structures protected
protected with
with
intumescent coating
coating is based on the standard fire resistance test, described before (EN
13381-8). Based on these results, tables that list the minimum dry film thickness (DFT) of
the product required for achieving a certain
certain fire
fire resistance
resistance in
in terms
terms of
of time
time are
are provided.
provided.
In this way, the structural fire engineer can design or assess the fire resistance of the steel
element protected with IC in a very simple way. In Figure 7, the main steps steps are
are described.
described.

Figure 7. The
Figure 7. The main
main step
step for
for designing
designing IC thickness.
IC thickness.

The Annex E of EN13381-8 describes another method to assess and design the fire
resistance of steel structures protected with IC by using the effective thermal conductivity.
This empirically informed procedure is called the “variable λ method”. It derives from an
energy balance taken during a given time interval during heating for unidirectional heat
flux conditions. This method is intended for evaluating the equivalent thermal conductivity
of fire protection systems and is defined by the following expression:

V 1
λ IC = d IC × × ca × ρa × × ∆θ a,t (1)
Ap (θt − θ a,t ) × ∆t

where:
dIC = dry film thickness of reactive product, in meters;
V/Ap = inverse of the steel section factor, in meters;
ca = temperature-dependent specific heat capacity of steel at θa, in J/kgK;
ρa = density of the steel, in kg/m3 ;
θ t = furnace temperature, in Celsius degrees;
θ a,t = steel temperature, in Celsius degrees;
∆t = time step, in seconds;
where:
dIC = dry film thickness of reactive product, in meters;
V/Ap = inverse of the steel section factor, in meters;
ca = temperature-dependent specific heat capacity of steel at θa, in J/kgK;
ρa = density of the steel, in kg/m3;
Coatings 2022, 12, 696 θt = furnace temperature, in Celsius degrees; 10 of 17
θa,t = steel temperature, in Celsius degrees;
Δt = time step, in seconds;
Δθa,t∆θ
= steel temperature
= steel increase
temperature overover
increase timetime
stepstep
Δt, in
∆t,Kelvin degrees.
in Kelvin degrees.
a,t
Figure
Figure8 shows thethe
8 shows typical
typical development
developmentofofthe the IC
IC thermal conductivitycalculated
thermal conductivity calculatedboth
bothwith
withequation
equation11and andwith
withsimplified
simplified law,
law, as
as suggested
suggested by by de Silva et al. [25–27].Start-
de Silva et al. [25–27]. Starting
ing from
fromaathermal
thermalconductivity
conductivity very similar to the steel one (λs ), (λ
very similar to the steel one thes),ICthe
oneICreaches
one reaches a
a minimum
minimum value, and after it seems to stabilize. Knowing the thermal conductivity
value, and after it seems to stabilize. Knowing the thermal conductivity of the IC allows for of the
IC allows for the assessment
the assessment of the behaviour
of the behaviour of thesteel
of the protected protected steelusing
elements elements using bothand
both simplified
simplified
advanced andcalculation
advanced calculation methods. the
methods. However, However,
effectivethethermal
effective thermal conductiv-
conductivity of IC is not
ity of
only ICtemperature
is not only dependent.
temperature dependent.
Indeed, Indeed, asbydemonstrated
as demonstrated by researchers
researchers [15,26,27], it can also
[15,26,27], it can also be dependent on the rate of heating, the steel section
be dependent on the rate of heating, the steel section factor, the intumescent coating factor, the intu- dry
mescent coating dry film thickness, and nonuniform temperature distribution
film thickness, and nonuniform temperature distribution within the intumescent coatings. within the
intumescent coatings. These effects on the steel element temperature
These effects on the steel element temperature can be observed by analyzing Figure can be observed by 9,
analyzing
obtained Figure
from9,anobtained from campaign
experimental an experimental
presentedcampaign
in [15]. presented
In particular, in [15].
it canInbepartic-
observed
ular,that
it can
when be observed
setting thethat whenfactor,
section settingthethe section
higher factor, the was
temperature higher temperature
recorded in the was
sample
recorded in the
protected bysample protected
the smaller by the smaller IC thickness.
IC thickness.

λIC λIC_ variable λ method


λS λIC_ simplified law

θ (°C)

Coatings 2022, 12, x FOR PEER REVIEWθactivation θλ,min 700°C 11 of 18

Figure
Figure IC thermal
8. IC8.thermal conductivity
conductivity calculated
calculated withwith accurate
accurate (EN(EN 13381-8)
13381-8) and and simplified
simplified laws.
laws.
1000 dIC=1000µm 1000
θ (°C) θ (°C) A/V=125 m−1
900 900

800 800
A/V=250 m-1−1 A/V=125
A/V=125 m-1m
−1
A/V=250 m
700 700 1000µm

600 600
A/V=67
A/V=67 m-1m−1 500µm 1500µm
500 500

400 400 2000µm

300 300
ISO 834 ISO 834
M.θ.S._UNPROTECTED_250 Gas temperature
200 M.θ.S._UNPROTECTED_125 200
M.θ..S._1_2
M.θ.S._UNPROTECTED_67 M.θ.S.._3_4
M.θ.S.._3_4 100
100 M.θ.S.._5_6
M.θ.S._11_12
M.θ.S._19_20 M.θ.S.._7_8
0 0
0 10 20 30 40 50 60 70 80 0 10 20 30 40 50 60 70 80
t (min) t (min)

Figure9.9.The
Figure Thetemperature
temperatureevolution
evolutionininsteel
steelsamples.
samples.

4.2.
4.2.Design
Designand
andVerification
VerificationMethods
Methodswith
withaaPerformance-Based
Performance-BasedApproach
Approach
The new knowledge in the field of fire safety engineering
The new knowledge in the field of fire safety engineering (FSE) is directing
(FSE) the current
is directing the cur-
regulations
rent regulations towards performance-based design. The design flexibility of thiscan
towards performance-based design. The design flexibility of this approach ap-
proach can enable the consideration of a safe and economical solution for the design of
eventual fire protection for structures. Indeed, with this approach, natural fire curves are
considered, according with the intended use of each part of the structure, geometry, ven-
tilation, and distribution of the fire loads, in order to obtain fire scenarios and fire curves
0 0
0 10 20 30 40 50 60 70 80 0 10 20 30 40 50 60 70 80
t (min) t (min)

Figure 9. The temperature evolution in steel samples.

4.2. Design and Verification Methods with a Performance-Based Approach


Coatings 2022, 12, 696 11 of 17
The new knowledge in the field of fire safety engineering (FSE) is directing the cur-
rent regulations towards performance-based design. The design flexibility of this ap-
proach can enable the consideration of a safe and economical solution for the design of
enable the consideration of a safe and economical solution for the design of eventual fire
eventual fire protection for structures. Indeed, with this approach, natural fire curves are
protection for structures. Indeed, with this approach, natural fire curves are considered,
considered, according with the intended use of each part of the structure, geometry, ven-
according with the intended use of each part of the structure, geometry, ventilation, and dis-
tilation, and
tribution distribution
of the fire loads, of
in the firetoloads,
order obtaininfire
order to obtain
scenarios andfire
firescenarios
curves asand fire curves
representative
as representative as possible of the potential fire of the
as possible of the potential fire of the compartment (Figure 10). compartment (Figure 10).

1200 ϑθ [°C]
(°C) ISO 834
1100 NATURAL FIRE CURVES

1000

900

800

700

600

500

400

300

200

100
t t[min]
(min)
0
0 15 30 45 60 75 90 105 120

Figure 10.
Figure 10. Natural
Natural fire
fire curve
curve compared
comparedwith
withthe
theISO834
ISO834one.
one.

As
As Figure
Figure1010shows,
shows,natural
naturalfirefirecurves
curvescancanbebevery different
very differentfromfromthethe
ISO834 standard,
ISO834 stand-
and
ard,these differences,
and these especially
differences, in the growth
especially in the phase
growth ofphase
the fire,
ofcan
theinfluence
fire, can the behaviour
influence the
of the reactive
behaviour protections,
of the such as the intumescent
reactive protections, such as the coatings, as demonstrated
intumescent by numerous
coatings, as demonstrated
researchers
by numerous [15,28]. This strongly
researchers [15,28].indicates
This stronglythat it is not applicable
indicates to extrapolate
that it is not applicable to theextrap-
value
of thermal properties, such as the thermal conductivity of IC obtained
olate the value of thermal properties, such as the thermal conductivity of IC obtained in accordance with
in
the fire exposure condition in the current assessment method [EN 13381-8],
accordance with the fire exposure condition in the current assessment method [EN 13381- to applications
under different fireunder
8], to applications exposures. Since
different fireitexposures.
is impossible to assess
Since fire-resistance
it is impossible ratings
to assess for
fire-re-
intumescent-coating-protected structural steel withstructural
sistance ratings for intumescent-coating-protected an infinitesteel
number
with ofancombinations
infinite numberof
parameters in a performance-based fire-resistance approach, it is crucial to characterize the
fire performance of intumescent coating in different fire exposures and structure designs.
In actual technical regulations, this topic is generally not yet addressed, but in some
countries, such as Italy, guidelines and technical references have been issued. Indeed, the
DCPREV 9962 [29], enacted in July 2020, clarifies the use of fire protections with natural
fire curves, prohibiting the design and assessment of steel elements protected with IC, as
their behaviour under natural curves is unknown both in terms of thermal and mechanical
properties (e.g., adhesion); this severely limits the adoption of FSE. In addition, in the
FSE approach, advanced calculation methods are usually used for thermo-mechanical
analyses and all the thermal properties have to be known including their variation with
temperature. Right here, a problem arises; indeed, this variation is known only with
standard fire curves used during the certification process in accordance with UNI EN
13381-8 as described before.
Even if numerous researchers have studied the behaviour of ICs under fire curves
different from the nominal ones, it is clear that the problem of designing and assessing
protected steel element by means of a performance-based approach is still open and more
research is needed in order to generalize a common methodology for identifying the IC
temperature-dependent thermal properties.
fire curves used during the certification process in accordance with UNI EN 13381-8 as
described before.
Even if numerous researchers have studied the behaviour of ICs under fire curves
different from the nominal ones, it is clear that the problem of designing and assessing
protected steel element by means of a performance-based approach is still open and more
Coatings 2022, 12, 696 12 of 17
research is needed in order to generalize a common methodology for identifying the IC
temperature-dependent thermal properties.

4.3.
4.3. Control
Control of
of IC
IC Application
For its
For its nature,
nature, the fire behaviour
behaviour of ofIC
ICmainly
mainlydepends
dependson ondry
dryfilmfilmthickness
thickness (DFT),
(DFT),
adhesion during
adhesion during normal and and fire
fire situation,
situation,andandswelling
swellingreaction
reactionininfire
firesituations.
situations.There-
There-
fore,in
fore, inorder
order to to obtain
obtain a full characterization
characterizationof ofthese
theseprotections,
protections,several
severaltests
testshave
havetoto
bebe
performedbefore
performed beforeandandafter
afteritsits application.
application. AllAll
thethe surface
surface properties
properties are are generally
generally as-
assessed
sessed according
according to several
to several techniques,
techniques, which which aredescribed
are well well described
in [25].in [25].
While in
While in the
the case of ICs, thethe UNI
UNI10898-1
10898-1[30]
[30]establishes
establishesthe
themethods
methodsfor controlling
for controlling
the application
the application of ofIC
ICsystems,
systems, suitable
suitablefor for
checking theirtheir
checking compliance with the
compliance project
with the spec-
project
ifications, drawn up in operation of the element to be protected and
specifications, drawn up in operation of the element to be protected and the degree of the degree of fire
fire
resistance required (Figure
resistance required (Figure 11).

Control of IC application
UNI 10898-1

Thickness Adhesion
UNI EN 2808 UNI EN ISO 4624

Wet FT Dry FT Dry FT


Assessment methods: Assessment methods: Assessment methods:
• mechanical; • mechanical; Cross-cut test instrument
• gravimetric • gravimetric
• photothermal. • optical;
• magnetic;
• radiological;
• photothermal;
Coatings 2022, 12, x FOR PEER REVIEW • acoustic. 13 of 18

Figure11.
Figure 11. Methods
Methods for assessing the
the correct
correct IC
ICapplication.
application.
The thickness consistency of the IC applied on an element can be measured according
The thickness consistency of the IC applied on an element can be measured according
to UNI EN 2808 [31], which contains several methods for determining both the wet-film
to UNI EN 2808 [31], which contains several methods for determining both the wet-film
and dry-film thicknesses of generic coatings applied to a steel substrate.
and dry-film thicknesses of generic coatings applied to a steel substrate.
The wet-film thickness has to be measured both during and immediately after apply-
The wet-film thickness has to be measured both during and immediately after applying
ing the IC in order to verify the uniform application of each layer of the IC and the overall
the IC in order to verify the uniform application of each layer of the IC and the overall
thickness. To measure the wet-film thickness, several alternative methods are suggested
thickness. To measure the wet-film thickness, several alternative methods are suggested
by UNI EN 2808 (see Figure 11). One of the most common methods is the use of a comb
by UNI EN 2808 (see Figure 11). One of the most common methods is the use of a comb
gauge, consisting of a flat plate made of a corrosion-resistant material with teeth along its
gauge, consisting of a flat plate made of a corrosion-resistant material with teeth along its
edges (see Figure 12).
edges (see Figure 12).

Figure
Figure 12.
12. Example
Exampleof
ofaacomb
combgauge.
gauge.

The reference teeth at the corners of the plate define a baseline along which the inner
teeth are arranged to give a graduated series of gaps. Each tooth is labeled with the as-
signed gap value.
With commercially available comb gauges, the maximum thickness that can be meas-
Coatings 2022, 12, 696 13 of 17

The reference teeth at the corners of the plate define a baseline along which the inner
teeth are arranged to give a graduated series of gaps. Each tooth is labeled with the assigned
gap value.
With commercially available comb gauges, the maximum thickness that can be mea-
sured is typically 2000 µm and the smallest increment is typically 5 µm.
After drying of the IC, it is necessary to check that the measured dry-film thickness is
equal to the designed one as well as the uniformity of the IC application. In addition, in
this case, the UNI EN 2808 suggests a series of measuring methods, which are summarized
Figure 11. Among the suggested methods, two widely used ones are acoustic (ultrasonic
thickness gauge) and optical instruments. The first type identifies the coating thickness
by measuring the propagation time of the waves through the layer to be measured up
to the steel substrate. Noninvasiveness and high precision are the advantages of using
this instrument; moreover, the new generation ones are very simple to use, also in situ,
after the application of the IC to the steel elements. The optical instrument allows for a
direct measurement of the thickness up to the steel substrate via a slight cut on the painted
surface. The blades are normalized, and the thickness can be obtained directly by reading
the value through a graduated microscope. The instrument is slightly invasive, and it
Coatings 2022, 12, x FOR PEER REVIEW 14 o
can be considered a good tool to check the measurements obtained by the ultrasonic one
(Figure 13).

Figure
Figure 13.13. Example
Example of DFT
of DFT measurement
measurement gauges.gauges.

Another
Another important
important parameter
parameterfor the
forIC is IC
the theisadhesion to the to
the adhesion steel
thesupport and
steel support and
the compatibility between the layers of the protective package (i.e., primer,
compatibility between the layers of the protective package (i.e., primer, coating, and t coating, and
topcoat), which can be assessed according to UNI EN ISO 4624 [32]. In particular, the
coat), which can be assessed according to UNI EN ISO 4624 [32]. In particular, the m
minimum tensile force necessary to detach the IC from the steel surface (adhesive failure) or
mum
the tensile
weakest layerforce
of thenecessary
IC system fromto detach theones
the other IC (cohesive
from thefailure)
steel surface
has to be(adhesive
measured. failure
thenature
The weakest layer of theofIC
and preparation thesystem from
substrate andthe
the other
IC typeones
may(cohesive failure)
influence the has to be me
test results.
ured.
Then, The
it is naturetoand
necessary referpreparation
to standardizedof the substrate
procedures (seeand the14).
Figure IC The
typemain
maysteps
influence
for the
results.
the Then,and
preparation it isexecution
necessary to refer
of the to summarized
test are standardized procedures (see Figure 14). The m
below:
• steps
Stepfor the preparation
(a)—surface and to
preparation: execution
guaranteeof thethe testbetween
bond are summarized
the dolly andbelow:
the coating,
• degrease the dolly andpreparation:
Step (a)—surface the area of thetocoating to be the
guarantee tested using
bond alcohol or
between theacetone to the co
dolly and
remove any oil, moisture, or dust;
ing, degrease the dolly and the area of the coating to be tested using alcohol or a
tone to remove any oil, moisture, or dust;
• Step (b)—application of adhesive: It must have cohesive and fixing properties grea
than those of the coating under test in order to obtain a failing of the coating. T
Coatings 2022, 12, 696 14 of 17

• Step (b)—application of adhesive: It must have cohesive and fixing properties greater
than those of the coating under test in order to obtain a failing of the coating. The
dolly should be gently pushed down to squeeze out excess adhesive and remove it
from around the edges of the dolly (Figure 14). Finally, wait the necessary time for the
adhesive to dry;
• Step (c)—separation of test area: after the adhesive dries, before starting the test, the
paint around the dolly should be removed to isolate a specific diameter test area.
Generally, a drill with a diameter approximately 1 mm larger than the diameter of the
dolly can be used;
• Step (d)—load application: The contact between the dolly and the actuator should be
Coatings 2022, 12, x FOR PEER REVIEW 15 of 18
carefully checked (Figure 14). The force must be applied perpendicularly to the plane
of the coated support at a uniform speed, less than approximately 1 MPa/s.

Figure 14.
Figure 14. Example
Exampleof
ofDFT
DFTmeasurement
measurementgauges.
gauges.

Both
Both thickness
thicknessand
andadhesion
adhesiontests,
tests,for
forthe
thecontrol ofof
control thethe
ICIC
application
application(UNI 10898-
(UNI 10898-
1),
1), have to be carried out on several points of the element according to its shape (see(see
have to be carried out on several points of the element according to its shape Figure
Figure 15).measuring,
15). After After measuring, the conditions
the conditions of acceptability
of acceptability have have
to beto be satisfied
satisfied according
according to UNI
to UNI
10898-1.10898-1.

Control of IC application
UNI 10898-1

Thickness Adhesion

H shape profile 6 points 3 points

Square profile
4 points 2 points

Tube profile
4 points 1 point
Figure 14. Example of DFT measurement gauges.

Both thickness and adhesion tests, for the control of the IC application (UNI 10898-
Coatings 2022, 12, 696 1), have to be carried out on several points of the element according to its shape (see 15
Figure
of 17
15). After measuring, the conditions of acceptability have to be satisfied according to UNI
10898-1.

Control of IC application
UNI 10898-1

Thickness Adhesion

H shape profile 6 points 3 points

Square profile
4 points 2 points

Tube profile
4 points 1 point

Plane element
5 points 2 points

Corrugated element

6 points 3 points
Figure 15.Measurement
Figure15. Measurementpoints
pointsfor
forchecking.
checking.
5. Conclusions
Intumescent coating is one of the most common materials for protecting steel structures
from fire. Its particular nature of reactive material causes a thickness variation during
the thermal transience with a decrease in its thermal conductivity. Even if this material
is well studied in the literature from the chemical and physical points of view, a lack of
information is sometimes found in the field of certification and design. Indeed, on one hand,
the development of new products with always higher fire performance are required from
the protection market; on the other hand, these protections should be compliant with the
fire safety engineering approach in which natural fire curves are required. Therefore, the
main objective of this paper was to provide a comprehensive overview of the certifications,
design, and control of application procedures for the correct approach to the use of these
fire protections, especially in Italy.
The qualification process of all materials and products employed for structural use is
mandatory in Italy. Provided that performance assessment of IC systems is not covered
by any harmonized standard, their quality certification can be pursued through a national
assessment procedure, regulated by indications of the National Fire and Rescue Service
by means of EN 13381-8:2013 or a European assessment procedure. The latter consists
of a voluntary certification process to be undertaken with the guidance of a TAB and
finally achieving the release of an ETA on the basis of EAD 350402-00-1106, i.e., a product
code concerning the performance assessment of reactive coatings for fire protection of
steel elements.
Regarding the IC design and control of application procedures, it emerges that:
- The data provided by manufacturers allow for application on only a prescriptive-
based approach, obtaining, trough tabular data, the IC thickness necessary for a given
structural element to reach a required fire resistance time;
- Generally, no information is provided about the thermal properties of these materials;
- According to EN 13381-8, a variable thermal conductivity can be calculated starting
from the experimental results, allowing to assess the behaviour of the protected steel
Coatings 2022, 12, 696 16 of 17

elements using both simplified and advanced calculation methods if the ISO834 curve
is used;
- The voluntary application regulations describing the control of intumescent coating
application are often ignored and not applied.
Another important conclusion is that, at the moment in Italy, to model steel structures
protected with intumescent coating is forbidden if the modern fire safety engineering ap-
proach is used, because not much information is available on the behaviour of intumescent
systems under natural fire curves. Therefore, it is necessary to carry out experimental tests
in order to investigate the performance of the intumescent coating under fire curves with
different heating rates in order to identify a common methodology for the definition of IC
temperature-dependent thermal properties.

Funding: This research received no external funding.


Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

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Applicativi; Ministero dell’interno—Dipartimento dei Vigili del Fuoco, del Soccorso Pubblico e Della Difesa Civile. Direzione
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30. UNI 10898-1; Fire Proofing Systems—Inspection Modes for the Installation—Part 1: Intumescent Coating. UNI: Milano, Italy, 2012.
31. EN 2808; Paint and Varnishes—Determination of Film Thickness. CEN-CENELEC Management Centre: Brussels, Belgium, 2007.
32. EN ISO 4624; Paint and Varnishes—Pull-Off Test for Adhesion. CEN-CENELEC Management Centre: Brussels, Belgium, 2006.

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