Ind. Eng. Chem. Res.

2006, 45, 7475-7481 7475

High-Throughput Fire Testing for Intumescent Coatings

M. Jimenez, S. Duquesne, and S. Bourbigot*
Laboratoire des Procédés d’Elaboration de ReVêtements Fonctionnels (PERF), LSPES UMR 8008, Ecole
Nationale Supérieure de Chimie de Lille, BP90108, F-59652 VilleneuVe d’Ascq, France

A new small-scale fire test is described in this paper. The goal was to design a high-throughput test permitting
the optimization of intumescent mastic coatings formulated to protect steel in the case of hydrocarbon fire.
This type of coating, applied on steel plates, beams, or columns, is usually evaluated in large industrial furnaces.
Such experiments are expensive and time-consuming. The development of a small-scale laboratory test using
an external heat flux is investigated. Temperature as a function of time is recorded on the back of the coated
steel panel. It is shown that temperature profiles are very well correlated with those measured in industrial
furnaces. This low-cost and fast test is very repeatable, and it allows rapid screening of a large number of
different coating formulations. The test also shows good correlation with the results obtained in cellulosic
fire testing.

1. Introduction as petrochemical complexes and offshore platforms, with a

The protection of metallic materials against fire has become
an important issue in the construction industry. Indeed, preven-
tion of the structural collapse of the building is paramount to
ensure the safe evacuation of people from the building, and is
a prime requirement of building regulations1 in many countries.
Steel usually begins to lose its structural properties above 500
°C. Intumescent coatings are designed to perform under severe
conditions and to maintain the steel integrity for between 1 and
3 h in some cases when the temperature of the surroundings is
in excess of 1100 °C.2-4 Upon heating, foamed cellular charred
layers are formed on the surface, which protect the underlying
material from the action of the heat and/or flame.
Different types of fire curves, corresponding to different
standards, can be used during industrial tests, the main ones
being cellulosic and hydrocarbon fire test curves,5,6 as shown
in Figure 1.
The cellulosic fire test curve (ASTM E-119) intends to
simulate the rate of temperature increase that can be observed
in a residential or commercial building fire where the main
sources of combustion fuel are cellulosic in nature, such as
wood, paper, furniture, and common building materials. The
fire curve is characterized by a relatively slow temperature rise
to around 927 °C after 60 min. But although this fire curve is
still used, it is noteworthy that the burning rates for certain
materials, e.g., petrol gas and fuels, etc., are much larger than
the rate at which, for instance, timber would burn. As such,
there was a need for an alternative exposure for the purpose of
carrying out tests on structures and materials used within the
petrochemical industry, and thus the hydrocarbon curve was
developed.
The hydrocarbon test curve (UL1709) intends to simulate or
to be indicative of the rapid temperature rise measured when a
hydrocarbon fuel such as oil or natural gas burns: the temper-
ature rises rapidly to 1000 °C within 4 min until reaching
temperature between 1100 or 1200 °C.
This hydrocarbon fire test curve, developed by the Mobil Oil
Co. in the early 1970s and adopted by a number of organizations,
is now a well-accepted reference in high-risk environments such
* To whom correspondence should be addressed. Tel.: + 33 (0)3
20 43 48 88. Fax: +33 (0)3 20 43 65 84. E-mail: serge.bourbigot@
ensc-lille.fr.
10.1021/ie0608410 CCC: $33.50 © 2006 American Chemical Society
Published on Web 09/28/2006
typical rating of 2 h. This hydrocarbon test curve is also used
to simulate jet fire scenarios in which leaking high-pressure
hydrocarbon gases ignite to produce intense, erosive jet flames
that can reach speeds of 150 m/s. A standard jet fire test,
denominated OTI 95 634, has been developed jointly by the
U.K. Health and Safety Executive and the Norwegian Petroleum
Directorate for use predominantly on offshore installations.7 The
test impinges the high-speed stream of ignited propane fuel onto
a substrate coated with the product.8 The propane is delivered
at a rate of 0.3-20 kg/s, depending on the test site setup, and
can consume 1 ton of fuel/min.
The industrial test taken as reference in this paper is test
UL1709, and the intumescent formulations used in this study
are thick-film intumescent systems, designed to provide protec-
tion of steel in both hydrocarbon and jet fires. Intumescent thick
films are usually based on epoxy, vinyl, or other elastomeric
resins and contain ingredients providing intumescence upon
heating. They are available as solvent-free systems, permitting
the application of up to 8-10 mm thick coating.9-12 They are
hard and durable, and some of them can provide excellent
protection from corrosion.13,14 They exhibit very high adhesion
to the substrate and resistance to impact, abrasion, and vibration
damage. High tensile and compressive strengths can be obtained,
and weather resistance is excellent.
These intumescent coatings are high-value products for
industries, and the competition in developing new products is
high. But the development of new intumescent coatings depends
on many parameters: the intumescence concept15-18 requires a
balance between the fire properties and the level of additives
in the material. The formulation of the coating has first to be
optimized in terms of physical and chemical properties (char
strength, expansion, and viscosity, etc.) in order to form an
effective protective char.19 This latter should limit both the heat
transfer from the heat source to the substrate and the mass
transfer from the substrate to the heat source, resulting in
conservation of the underlying material. The formulations are
then evaluated in an industrial furnace using UL1709,20 in order
to compare their ability to protect the steel substrate from fire.
In a typical fire test, steel substrates coated with intumescent
coating are tested. Thermocouples are attached to the isolated
back of the plate, and the evolution of temperature is plotted
against time (Figure 2).
7476 Ind. Eng. Chem. Res., Vol. 45, No. 22, 2006
Figure 1. Main standard fire test curves.
Figure 2. Example of time/temperature curve registered.
The key parameter of this test is when the nonheated side of
the steel plate reaches 400 °C: the critical temperature of the
steel is an essential parameter; this parameter is defined as the
temperature at which only 60% of the original strength remains,
the point at which failure is imminent under full design loads.
It is important to take into account the load of the structure: if
the steel member is part of the main structure, it follows that
the load also needs to be considered when determining the
protection requirements. For regular reinforcing steel, the critical
temperature is 538 °C, while for prestressing steel bars, which
are made of high-carbon, cold-drawn steel instead of low-carbon,
hot-rolled steel, the critical temperature is significantly lower
at 427 °C. It is the reason 500 °C has been selected as a standard
for normally loaded structural components, while 400 °C has
been selected as a standard for heavily loaded structural
components such as, for example, offshore platforms.
Figure 3. Industrial furnace.
This temperature is known as the “failure temperature”. The
corresponding time is called the “time of failure”. The most
efficient coatings are the ones having the longest time of failure.
These furnace tests are however very expensive, and panel
preparation is time-consuming; moreover only a few panels can
be tested in 1 day. This is why small-scale and high-throughput
tests should be developed to allow rapid screening of formula-
tions21 and accelerate the research on new and more efficient
intumescent formulations. The test we have developed in our
laboratory tries to evaluate very rapidly the heat barrier effect
of intumescent coating when exposed to a heat flux.
Tests have been carried out on different intumescent epoxy-
based thick-film coatings: results and correlations are presented
and commented on in the first parts of this paper. The last part
of the paper discusses results also measured on cellulosic
intumescent coatings as test materials.
2. Experimental Apparatus and Methods
2.1. Industrial Fire Test. Industrial furnace tests have been
carried out in a 1.5 m3 furnace (Figure 3) according to UL1709.
The coatings are applied on a steel plate (thickness, 3.5 mm)
and cured for 1 week at room temperature. Thermocouples are
attached to the back of the coated plates. Five thermocouples
are used on each plate, so that an average temperature can be
obtained. The burning conditions try to fit as much as possible
the ramp of temperature of a hydrocarbon fire (about 200 °C/
min). Figure 4 shows the difference between the experimental

Figure 4. Comparison between standard and experimental hydrocarbon curves.
Figure 5. Four steel plates coated, before and after the test.
and the standard hydrocarbon curve. The main difference occurs
during the first minutes of heating: the increase of temperature
is much more rapid during the test compared to the standard.
This is not a problem, as the aim is to test the coatings under
the most severe conditions possible.
As four plates are tested at the same time, the plates are
isolated using glass wool. The plates are mounted vertically in
the furnace and burnt (Figure 5) until the thermocouples attached
to the back of the plates reach a temperature higher than 400
°C (the failure temperature).
Time/temperature curves are recorded, which characterize the
heat protective effect of the different coatings in a hydrocarbon
fire.
2.2. Small-Scale Test. Some small-scale tests such as the
cone calorimeter test,22 limiting oxygen index (LOI),23 and
flammability tests (UL94)24 already exist and are widely used
to evaluate different parameters of intumescent formulations,
for example, the heat release rate, the ignition time, and the
gases released, etc. By developing the current small-scale test,
the aim was to evaluate the efficiency of the intumescent coating
in terms of heat transfer. As in the large furnace test, the aim is
to obtain time/ temperature profiles measured on the back of
the coated steel plate.
The heat source is a heat radiator provided by Saint Gobain
(France). The steel plates used are squares of 5 × 5 cm2 and 5
mm thick; the steel is exactly the same as the one used in the
industrial test. About 1 mm of the intumescent coating is applied
on the surface of the steel plate. A black coating, provided by
Ind. Eng. Chem. Res., Vol. 45, No. 22, 2006 7477
Medtherm Corp. (Huntsville, Alabama), resistant to 800 °C and
having a constant emissivity of 0.92, is applied on the nonheated
side of the steel plates. The constant emissivity of the backside
of the plate allows accurate measurement of the surface
temperature of the plate using an infrared pyrometer. The
infrared pyrometer is positioned at a constant distance from the
steel plate, and the beam is pointed on the center of the plate.
It detects the temperature on the nonheated face of the steel
plate and registers the time/temperature curve on a computer.
This time however no failure temperature is considered, as the
heating temperature does not reach 1200 °C as in the large
furnace. This test is used mostly by comparing temperature
obtained after 20 min for one formulation to the test is shown
in Figure 6.
This small-scale test is very stable and repeatable. The
reference curve is the time/temperature curve obtained for the
virgin steel plate black-coated on its nonheated face.
The whole system is placed into a box in order to avoid the
effect of the fume cupboard: the aim is to reduce the convective
and chimney effects.
2.3. Materials. Different intumescent formulations have been
studied using both tests, to compare the results obtained. Because
all the formulations are provided by an industrial partner, the
identity of the components will not be given in this paper. Three
different types of formulations have been tested: the first type
comprised three basic intumescent epoxy-based formulations
(IF1, IF2, and IF3), which are compared to a reference
commercial intumescent mastic (IF4). The second series of tests
7478 Ind. Eng. Chem. Res., Vol. 45, No. 22, 2006
Figure 6. Presentation of the small-scale test.
Figure 7. Repeatability test on a virgin plate and on a virgin plate coated
with IF4.
were carried out on three intumescent epoxy-based mastics (IF5,
IF6, and IF7), also compared to the commercial formulation
(IF4). The final tests were carried out on three unknown
cellulosic coatings (IFA, IFB, and IFC), which have also been
Figure 8. (a) Industrial furnace and (b) heat radiator tests on five intumescent formulations.
tested in a large furnace using the cellulosic fire curve. The
purpose was to validate our test in different conditions.
3. Results and Discussion
3.1. Reproducibility Tests. Reproducibility tests were carried
out on the uncoated steel plate and on the steel plate coated
with 1 mm of the commercial reference IF4. The experiments
were performed on different days, and as it can be seen in Figure
7, the experimental reproducibility is very good in all cases
throughout the entire test.
3.2. First Series of Tests on “Basic” Formulations. Heat
radiator tests were first carried out on different formulations
(IF1, IF2, IF3, and IF4), and the results are compared with those
obtained in furnace tests. The formulations IF1, IF2, and IF3
are constituted by the main intumescent compounds of the
formulation IF4. The time/temperature curves obtained both at
the industrial furnace tests and with the heat radiator test are
shown in Figure 8a,b, respectively.
The time/temperature curves carried out in the industrial
furnace are shown up to 400 °C (failure temperature). The
parameter taken into account is the time of failure, namely, the
time when temperature reaches 400 °C. The materials exhibit
very different behavior: the most efficient coating is IF4 (time
of failure of about 40 min), while the worst one is IF1 (time of
failure of 10 min).
During the heat radiator test, there is an important increase
of temperature at the beginning of the test (from 0 to 350 s) in
all cases, but after 450 s the temperature remains quite steady.
If the temperatures reached at the end of the experiment are
compared, the best performance is obtained when the temper-
ature increases slowly during initial heating (t < 350 s) and
when the lowest temperature is reached at the end of the test (t
> 450 s). According to those observations, the curves can be
well-distinguished. The best formulation is still IF4 with a
temperature of about 320 °C reached at 1200 s, and the worst
one is still IF1, which reaches about 400 °C at 1200 s.
The ranking of results obtained after 1200 s in the heat
radiator test and at 400 °C in the furnace tests are then
summarized in Table 1.
The rank orders between the heat radiator test and the
industrial furnace agree well each other. So the heat radiator
test appears to be a very interesting tool to carry out an initial

Table 1. Ranking of Results Obtained for Tests on Intumescent
Formulations (1 w Best Result)
heat radiator test industrial furnace test
IF1 4 4
IF2 3 3
IF3 2 2
IF4 1 1
assessment of whether a coating might perform well in a
hydrocarbon fire. Another interesting facet of the heat radiator
test is that it is possible to look at the texture of the resulting
formed char to estimate its mechanical resistance. It is a major
advantage since an intumescent coating should also resist
external stresses and some prediction of the behavior on the
large scale might be done. Another observation we made during
the industrial furnace test is that the formulations IF1 and IF2
fell off the steel plate during the test. For this reason it was
decided to set up the same test with the coated plate mounted
vertically (Figure 9).
Figure 9. Small-scale test with the steel plate put vertically.
The same coating formulations were tested with this experi-
mental setup (Figure 10).
Figure 10. Tests carried out with plates mounted vertically.
As above, the temperature/time curves show that IF1 is the
least effective formulation. Nevertheless it is difficult to
determine which one of the three other formulations is the best
one, as they reach the same temperature after 1200 s.
First experimental observations show that there are more heat
losses on sides due to convective phenomena than when the
plates are mounted horizontally: the heat radiator is still at the
same distance from the plate, but the uncoated steel plate reaches
Ind. Eng. Chem. Res., Vol. 45, No. 22, 2006 7479
only 380 °C, whereas it reached 450 °C when the plate was
mounted horizontally. The second observation is that the
coatings swell less than in the first test and do not ignite. Those
comments explain then why this particular experimental setup
does not permit discrimination of the formulations. It is not our
goal here to compare further the two setups. Our initial aim
was to test the mechanical resistance of the char on plates and
see if formulations IF1 and IF2 fell off from the plate, as it
could be observed during furnace testing. However, the tem-
peratures should be too low here: the char, which does not swell
a lot, does not fall off the plate.
Considering that the curves are not very distinguishable and
that the char remains on the steel plate, the horizontal plate
system will be considered in the following part.
3.3. Second Series of Tests Carried out on Intumescent
Mastics. A second series of tests was carried out on four
different intumescent mastics: IF4 (reference formulation), IF5,
IF6, and IF7. Curves obtained in the industrial furnace and heat
radiator test are presented in Figure 11a,b, respectively.
The best formulation in the furnace evaluated up to 30 min
is IF5, and the worst formulation is IF7. After 30 min, the time/
temperature curve of the formulation IF5 crosses over the curve
of the formulation IF4, and at the end of the test, IF4 is still the
most efficient formulation.
Considering the results of the small-scale test, the best
performing formulation up to 13 min is IF5 and the worst is
IF7. Interestingly the same crossover of curves between IF5
and IF4 is subsequently observed: after 13 min the formulation
IF4 shows the best performance.
This crossover can be the consequence of different phenom-
ena: this can be due to changes in the structure of the char
(cracks, change of viscosity, bubbles, and mechanical strength
of the char) which modify the heat transfer between the
intumesced coating and the plate. Or some components inside
the coating, such as fibers, might provide an additional insulating
effect after a certain time of heating accumulating at the surface.
The ranking of results obtained after 1200 s with heat radiator
and at 400 °C in the furnace test are summarized in Table 2.
As above, the heat radiator and the industrial furnace tests
agree very well each other. It is noteworthy that the temperature/
time curves exhibit a similar behavior including the crossover.
According to those results, we may conclude that the heat
radiator test can be used to effectively rank the efficiency of
intumescent mastics.
However, there are not only intumescent epoxy mastics in
the fire protection coating market: two main kinds of coatings
exist, the thick-film intumescent coatings (mastic) and thin-film
intumescents (cellulosic coatings). The next part of the paper
will examine whether the heat radiator test can also be used to
evaluate cellulosic intumescent coatings.
3.4. Third Series of Tests Carried out on Cellulosic
Coatings. Thin intumescent films are used for protection from
cellulosic type fires. They are generally available as solvent-
or water-based systems and applied by spray or brush-roller in
thin-film coats up to 3 mm thick. They typically use thermo-
plastic acrylic based resin systems, and they intumesce quickly
when exposed to a cellulosic type fire environment. Protection
for 1 h can be achieved with 1-3 mm thick coatings. Thin
intumescent films are often referred to as “fire retardant paints”
rather than “fireproofing” materials due to their lower fire
resistance compared to thick intumescent films. Many of them
are unsuitable for exterior use unless a topcoat is applied over
them, and the test ratings are limited to cellulosic fires only.
Advantages of these products include that they are available in
7480 Ind. Eng. Chem. Res., Vol. 45, No. 22, 2006
Figure 11. (a) Industrial furnace and (b) heat radiator tests on four intumescent mastics.
Figure 12. (a) Heat radiator and (b) furnace tests on three intumescent cellulosic coatings.
Table 2. Ranking of Results Obtained for Intumescent Mastics (1 w
Best Result)
heat radiator test industrial furnace test
IF4 1 1
IF5 2 2
IF6 3 3
IF7 4 4
wide range of colors and they are inexpensive and relatively
easy to apply. They are mostly used inside buildings.
Testing of cellulosic coatings is different from testing
intumescent mastics: the hydrocarbon fire curve is replaced by
the standard cellulosic fire curve (Figure 1). During this test,
coatings can be applied on steel plates, or also on columns and
beams, which are put inside the furnace, and the standard
cellulosic fire is applied to them. As these coating are not
designed to be applied on heavily loaded components, 500 °C
is taken as the failure temperature, with the corresponding time
of failure.
Three commercial cellulosic coatings (IFA, IFB, and IFC)
are evaluated using the heat radiator and furnace tests. The
curves obtained for both tests are presented in Figure 12a,b).
This was a “blind test”, as nothing was known about the
composition of the coatings tested.
The heat radiator test gives three distinct curves: the coating
IFA shows much better efficiency than the other coatings. The
Table 3. Ranking of Results Obtained for Intumescent Cellulosic
Coatings (1 w Best Result)
heat radiator test industrial furnace test
IFA 1 1
IFB 3 3
IFC 2 2
difference between IFB and IFC is less clear; at the end of the
test IFC reaches a slightly lower temperature than IFB, but at
the start of the test (up to 3 min) IFC provides the better
performance
The furnace test shows distinct curves, the most efficient
formulation being IFA and the least efficient being IFB.
The rankings of results obtained at 1200 s with the heat
radiator and at 500 °C in the furnace tests are presented in Table
3.
As above, correlation between the two tests is excellent, with
the same ranking of coating performance obtained.
4. Conclusion
A reliable high-throughput test has been developed in the
laboratory in order to evaluate the heat barrier effect of different
intumescent formulations. This is a small-size, rapid, and low-
cost test, easy to use, showing great repeatability and allowing
rapid screening of thick- and thin-film intumescent formulations.

It can be used in two experimental configurations (plates
mounted vertically or horizontally), leading to complementary
results. It is a very interesting preliminary tool for the develop-
ment of new intumescent coatings as it can avoid the require-
ment to carry out large furnace tests on many coating formu-
lations. Only the promising formulations will be progressed to
full-scale furnace testing, saving both time and money. This
test can be used to study coatings on different substrates (steel,
aluminum).
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ReceiVed for reView June 30, 2006
ReVised manuscript receiVed August 21, 2006
Accepted August 23, 2006
IE0608410