Materials Today: Proceedings xxx (xxxx) xxx

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Materials Today: Proceedings

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A low smoke zero halogen zero phosphorous fire-retardant rubber

shroud
Sunita Mohapatra ⇑, Pallabi Sarkar, Ganesh Bhoye
Raychem Innovation Centre, Raychem RPG Pvt. Ltd., Halol, Gujarat 389350, India

a r t i c l e i n f o a b s t r a c t

Article history: This low smoke zero halogen composition was developed for a product called shroud. Shroud is used to
Received 11 March 2020 provide protection against dirt or foreign substance gathering on cable gland assembly. Mostly they pro-
Received in revised form 30 March 2020 vide mechanical impact resistance and serve as additional protection. The existing shroud is made up of
Accepted 28 April 2020
Polyvinylchloride (PVC). PVC is inherently a self-extinguishing fire-retardant material due to high con-
Available online xxxx
centration of chlorine (56.8%) in its chemical structure. However, due to environmental and health con-
cerns, an alternate material or formulation is required for shroud which should be non-halogenated
Keywords:
flame-retardant. In addition, the formulation should not generate very high smoke on combustion as
Low smoke
Silicone rubber
PVC does. Further, the required material should have service temperature of
60 °C to 200 °C. The present
Fire-retardant work describes a halogen free, phosphorous free, low smoke fire retardant rubber composition.
Zero halogen Ó 2020 Elsevier Ltd. All rights reserved.
Zero phosphorous Selection and peer-review under responsibility of the scientific committee of the International
Conference on Aspects of Materials Science and Engineering.

1. Introduction As halogen containing materials offers good fire-retardant prop-

A cable gland is a device used to attach and secure the end of an
electrical cable to the equipment as shown in Fig. 1. Cable glands
are designed for use with all types of electrical power, control,
instrumentation, data telecommunications cables & fire rated
Cables [1]. They are used as a sealing and termination device to
ensure that the characteristics of the enclosure which the cable
enters can be maintained adequately. Cable glands are made up
of mostly brass, aluminum, copper and galvanized steel.
A shroud is an elastomeric sleeve and is required to use with all
cables glands to provide additional ingress protection and to min-
imize the risk of dust or any other foreign substance to accumulate
around cable gland body. The shroud is an insulation material and
in addition, it should be fire-retardant with UL-94V0 rating and
should have working temp from
60 °C to + 200 °C.
The shroud is like a cylindrical sleeve with a conical portion
forming an arrow shape. During installation of shroud, the arrow
end of the sleeve is cut with a knife, enabling it to be slipped over
a wide range of cable diameters and assists ease of installation. At
the other end, it slips-on the periphery of the cable gland as shown
in Fig. 2.
⇑ Corresponding author.
E-mail address: sunita_mohapatra@raychemrpg.com (S. Mohapatra).
erties, the existing shroud is Polyvinyl chloride (PVC) based. PVC is
inherently a self-extinguishing fire-retardant material due to high
concentration of chlorine (56.8%), a halogen element in its chemi-
cal structure. However, these shrouds on combustion produce lots
of smoke containing HCl (hydrogen chloride). These gases are very
toxic and corrosive. Further, as these shrouds produce lots of
smoke, they obscure the visibility to make it difficult to escape in
case of fire. Hence, these polymers are not safe to use where the
protection of people and equipment is critical. Apart from this, to
achieve flame retardant properties in polymers halogen containing
additives (bromine and/or chlorine containing) are frequently used
as these are very cost-effective. However, halogens are highly reac-
tive and harmful, as they can form toxic and corrosive gases. Fig. 3
shows the halogen elements in the periodic table.
Phosphorous containing additives e.g. phosphates are also being
used as replacement of halogenated fire retardants. This class cov-
ers a wide range of both inorganic and organic compounds e.g.
phosphate esters and various phosphates. Toxicological studies
have revealed potential neurological and carcinogenic effects of
these compounds. Hence both halogenated and phosphorous con-
taining flame-retardant polymers are toxic and not environment
friendly.
Few PVC based low smoke shrouds are also available which
contain additives to suppress the smoke, and they are marketed

https://doi.org/10.1016/j.matpr.2020.04.815
2214-7853/Ó 2020 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Conference on Aspects of Materials Science and Engineering.

Please cite this article as: S. Mohapatra, P. Sarkar and G. Bhoye, A low smoke zero halogen zero phosphorous fire-retardant rubber shroud, Materials Today:
Proceedings, https://doi.org/10.1016/j.matpr.2020.04.815
2 S. Mohapatra et al. / Materials Today: Proceedings xxx (xxxx) xxx

to quantify smoke produced during combustion) or Limiting oxy-

gen index etc data are not available explicitly.
In view of the limitations inherent in the available shroud mate-
rials, there exists a need for an improved fire-retardant rubber
composition for making the shroud which should generate very
low smoke and must be halogen free, phosphorous free. This paper
describes development of such kind of material formulation, which
is a fire-retardant with UL-94-V0 rating along with capable of serv-
ing with a temperature range of
60 °C to +200 °C and which can
be made in a simple, cost effective, reliable, secure and environ-
mentally friendly manner.

2. Experimental and material selection

2.1. Selection of the elastomer

The working temperature range for various elastomers is shown

in Fig. 4. As per the requirement, only elastomers viz. FKM, VMQ
and FVMQ could be considered as they have service temperature
from
60 °C to +200 °C.
Fig. 1. Cable gland connecting cable to the equipment. Further, the elastomer must be non-halogenated, thus FKM and
FVMQ could not be considered as both contain fluorine, a halogen

Fig. 2. Cable gland and Shroud assembly.

under the name ‘‘low smoke & fume” PVC shroud (LSF). However,
they still contain chlorine and generate toxic hydrogen chloride
gas on combustion. Moreover, the smoke generation is not margin-
ally suppressed with these kind of low smoke shrouds as observed
in the case of low smoke zero halogen ones.
LSZH (Low Smoke Zero Halogen) shrouds are low smoke pro-
ducing shrouds and they don’t contain halogen elements. However,
there is no mention of whether they contain any phosphorous or
not. Further, the smoke generation parameter (e.g. smoke density
Fig. 4. Working temperature for various elastomers.

Fig. 3. Halogen family in Periodic table.

Please cite this article as: S. Mohapatra, P. Sarkar and G. Bhoye, A low smoke zero halogen zero phosphorous fire-retardant rubber shroud, Materials Today:
Proceedings, https://doi.org/10.1016/j.matpr.2020.04.815
 S. Mohapatra et al. / Materials Today: Proceedings xxx (xxxx) xxx 3

element. Hence, the only elastomer suitable for this work is VMQ,
the vinyl silicone rubber. The grade used for this work has vinyl
content around 0.03–0.18% per mole and a hardness of 30 shore
A and specific gravity 1.10 g/cm3.
2.2. Selection of fire-retardant additives
A fire retardant is a substance that is used to slow or stop the
spread of fire or reduce its intensity. This is commonly accom-
plished by chemical reactions that reduce the flammability of fuels
or delay their combustion. Most of the fire-retardant additives are
either contain halogen and/or phosphorous. These additives are
abundantly available and are cost effective. Their performance is
also quite well, but these additives and their products are toxic
and corrosive as mentioned earlier in Section 1.
Hence the development of a non-halogenated and non-
phosphorous recipe for this product is a need of the hour. Hence
the ingredients are also chosen which are halogen and phospho-
rous free.
The fire-retardant and smoke suppressant fillers used in this
work are hydroxides of aluminium and magnesium i.e. commonly
known as Aluminium hydroxide (ATH) and Magnesium hydroxide
(MDH). These two fire-retardant additives used in this work are
non-halogenated and non-phosphorous. The These inorganic fillers
are getting increasing importance in the industry because of their
desirable combination of low cost, low smoke, and relatively high
fire-retardant efficiency.
The decomposition temperature of ATH begins at ca. 240 °C,
whereas MDH begins to decompose at 320 °C. ATH provides a
flame-retardant effect as it decomposes endothermically (DH –
1171 kJ/kg) into aluminum oxide and water (about 35 wt%) as
shown in Eq. (1).
2Al (OH)3! Al2 O3 + 3H2 O
Magnesium hydroxide, MDH also decomposes endothermically
(DH – 1372 kJ/kg) into magnesium oxide and water (about 31 wt%)
as shown in Eq. (2).
Mg (OH)2! MgO + H2 O
These decomposition reactions absorb heat from the combus-
tion zone and in addition, the resulting metallic oxide is left behind
and provides a protective intumescent layer on the surface of the
substrate. These two flame retardants promote charring and serve
as a barrier to heat and mass transfer. This contributes to extin-
guishing a flame.
2.3. Preparation of the specimen
The compounding or mixing was done in an internal mixer or
torque rheometer (Make: Harden Industries, China; Model: RTOI-
55/20). Roller rotors were used in the torque rheometer with a
rotor speed ratio of 2:3 to ensure a proper shear during mixing
of the additives in the VMQ rubber. The rubber and antioxidant
were mixed at a temperature of 80 °C to allow the antioxidant to
melt and to be well disperse the polymer matrix. Then other addi-
tives were added and processed for 3–4 min at 60 rpm to ensure
proper dispersion of all the fillers. The curatives were added at
the end and mixed for another 1 min. Care should be taken not
to rise the melt temperature in the internal mixer above 110 °C,
otherwise it may lead to scorch or premature vulcanization of
the rubber and this is not desirable.
The samples were molded at 170 °C in a hydraulic compression
machine. The specimens were prepared as per respective standards
for various tests viz. cure time, limiting oxygen index, smoke den-
sity test, flammability test UL-94V0 and UL-94 HB, break down
voltage and arc resistance etc.
2.4. Optimization of the curatives
Since the base elastomer for the system is Vinyl silicone rubber,
hence the suitable curing system is peroxide crosslinking. The
curatives used in the formulation were chosen to be dicumyl per-
oxide as the peroxide curing agent and triallyl cyanurate, TAC as
the coagent.
Six formulations were prepared as per Table 1. The weight of
the ingredients was expressed in terms of phr (parts per hundred
gram of rubber). The cure time of all the samples were evaluated
at 170 °C in an oscillating disc rheometer (Make: Alpha technolo-
gies; Model: ODR 2000) as per ISO 3417. The optimum cure time,
T90 of all the formulations were listed in Table1.
It is evident from Table 1 that, F1 and F2 has almost similar cure
ð1Þ time. This means that irrespective of the type of fire-retardant
additives i.e. ATH or MDH, the cure rate is same for both and so
as the cure time. Further, with decrease in the curing agent, the
cure time increases as shown from F1, F5 and F6. As this peroxide
curing is a free radical reaction, the more the curing agent, the
more the free radicals generated and available for curing; hence
the faster the cure rate which leads to lower cure time. The F3
ð2Þ
and F4 formulations contain 1 phr of antioxidant TDQ (2, 2, 4-
trimethyl-1, 2-dihydroquinoline). The antioxidants are used to
protect rubber articles against oxidative ageing and degradation.
However, antioxidants function follows free radical mechanism.
They act as scavenger for free radicals. Thus, in the peroxide curing
which also involves free radical mechanism, presence of antioxi-
dants reduces the cure rate and thus, a higher cure time.

Table 1
The Recipe and the Optimum cure time.

Sl no. Ingredients Sample Code

F1 F2 F3 F4 F5 F6
1 VMQ 100 100 100 100 100 100
2 TDQ – – 1 1 – –
3 silicone oil 0.4 0.4 0.4 0.4 0.4 0.4
4 Silane 0.2 0.2 0.2 0.2 0.2 0.2
5 Ppt Silica 5 5 5 5 5 5
6 ATH 40 – 40 40 40 40
7 MDH – 40 – – – –
8 DCP 1.5 1.5 0.8 0.5 0.8 0.5
9 TAC 0.4 0.4 0.3 0.2 0.3 0.2
Optimum Cure time (T90 in 1.32 1.47 5.67 7.03 1.83 2.08
minutes)

Please cite this article as: S. Mohapatra, P. Sarkar and G. Bhoye, A low smoke zero halogen zero phosphorous fire-retardant rubber shroud, Materials Today:
Proceedings, https://doi.org/10.1016/j.matpr.2020.04.815
4 S. Mohapatra et al. / Materials Today: Proceedings xxx (xxxx) xxx

A cure time of 5–10 min is ideal and acceptable in industry for

processing. Hence, for further work, the curatives, DCP 0.5 phr and
TAC 0.2 phr was considered.

2.5. The fire-retardant formulation development

In this work, a high quantity of the flame-retardant filler is

desirable to achieve better flame-retardant characteristic. How-
ever, a high quantity of such fillers generally poses a practical
problem in processing or mixing and thus, it becomes difficult to
achieve a homogenous dispersion. This ultimately leads to poor
properties of the final product. To ease in processing and achieve
uniform dispersion, additives like low molecular weight silicone
oil is used in this composition. Silicone oil helps in ATH and/or
Mg (OH)2 filler processing and homogenous dispersion in the
matrix. Further, precipitated silica was used as a reinforcing filler
in this composition. A silane coupling agent i.e. vinyl triethoxy
silane was used for silica filler dispersion in the rubber matrix
[2] . Six formulations were prepared as shown in Table 2.
All these formulations were evaluated for Limiting oxygen
index and smoke density. Apart from this, the formulations were
evaluated for flammability rating, halogen test and dielectric test.
3. Results and discussion
Fig. 5. Temperature Index Test (By extrapolation method).
composition with 100 phr ATH has highest LOI value of 42.8%,
which infers a high flame-retardancy behaviour.
Temperature Index (TI) is the temperature at which a specimen
will only just burn downwards in a candle-like manner in air (21%
oxygen). The aim is to find the minimum temperature required to
just sustain combustion of the sample in air. For this test, the oxy-
gen index value is determined at various temperatures and then
the data is extrapolated to oxygen index of 21% as shown in
Fig. 5. The sample with 100 phr ATH (SA3) was subjected to tem-
perature index test. The observed temperature index by extrapola-
tion method at 21% oxygen index was found to be more than
250 °C as shown in Fig. 5.

3.1. Limiting oxygen index (LOI) & temperature index (TI) test
All the compositions were evaluated for Limiting oxygen index
and temperature index as per ASTM D2863. All the samples are
molded into the dimension of 150 mm X 6.5 mm X 3 mm as per
the standard. The specimens were conditioned at 23 ± 2 °C and
50 ± 5% relative humidity for 88 h [3].
Limiting oxygen index (LOI) is the minimum concentration of
oxygen in an oxygen/nitrogen mixture in which the material will
burn. As air contains approximately 21% oxygen it is known in lit-
erature that a material with an oxygen index greater than about
26% will be self-extinguishing. Hence the higher the LOI value, bet-
ter will be the flame retardancy. The LOI values of the samples is
expressed in terms of percentage and is shown in Table 3.
From Table 3, it is evident that ATH has better flame retardancy
behaviour than magnesium hydroxide in silicone rubber. The
3.2. Smoke density test
This test method is used to measure the smoke producing char-
acteristics of polymers under controlled conditions of combustion
(as per ASTM D2843). The test specimen of size
25 mm  25 mm  6 mm is exposed to flame for a duration
4 min and the smoke is substantially trapped in the chamber [4].
The test chamber is instrumented with a light source, photo-
electric cell, and meter to measure light absorption horizontally
across the 300 mm light beam path. The measurements are made
in terms of the loss of transmission through a collected volume
of smoke produced under controlled conditions. The apparatus is
constructed so that the flame and smoke can be observed during
the test. Initially when no smoke is evolved the light absorbance
will be zero and when the sample starts burning the light is being

Table 2
The fire-retardant rubber recipe.

Sl no. Ingredients Sample Code

A1 A2 A3 M1 M2 M3
1 VMQ 100 100 100 100 100 100
2 TDQ 1 1 1 1 1 1
3 silicone oil 0.4 0.5 0.6 0.4 0.5 0.6
4 Silane 0.2 0.2 0.2 0.2 0.2 0.2
5 Ppt Silica 5 5 5 5 5 5
6 ATH 40 70 100 0 0 0
7 MDH 0 0 0 40 70 100
8 DCP 0.5 0.5 0.5 0.5 0.5 0.5
9 TAC 0.2 0.2 0.2 0.2 0.2 0.2

Table 3
LOI and Smoke density rating.

Test Sample Code

A1 A2 A3 M1 M2 M3
LOI, % 29.8 35.7 42.8 24.6 26.2 29.2
Smoke density rating, % 34.5 27.6 19.3 41.3 39.5 39.5

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 S. Mohapatra et al. / Materials Today: Proceedings xxx (xxxx) xxx
Fig. 6. Smoke Density Test: Reading of light absorption at 15 s interval.
obstructed by the smoke and the light absorbance increases. The
percent of light absorbed is being recorded for every 15 s through-
out the total 4 min duration. The smoke density of the sample is
directly proportional to the light absorbance measured. The time
taken by the sample to burst into flame and the behavior of sample
such as melting, dripping, foaming or charring can also be noted.
The light absorbance data is plotted against the time as shown
in Fig. 6. It is observed from Fig. 6 that, ATH samples have compar-
atively lower light absorbance than magnesium hydroxide in sili-
cone rubber. Moreover, the composition with 100 phr ATH has
the lowest light absorbance, which means 100 phr of ATH in sili-
cone rubber generates very low smoke. The maximum smoke den-
sity of the sample is the highest point on the curve. The total smoke
produced by the sample is given by the area under the smoke
curve. The smoke density rating represents the total smoke present
in the chamber for the 4-minute time interval. Hence Smoke Den-
sity rating, is the ratio between area under the curve & total area of
the graph.
To qualify for low smoke criteria, the smoke density rating
should be less than 60% [5] as per the industry standard. A value
of smoke density more than 60% is not acceptable as it will obscure
the visibility. The smoke density rating (%) was measured and
listed in Table 3. It is seen that. all the formulations have smoke
density rating less than 60%. Further, ATH samples have lower
smoke density rating than MDH samples. This means ATH samples
will generate low smoke in comparison to MDH samples. The com-
position with 100 phr ATH has smoke density rating of less than
20%. Moreover, charring was observed in all the samples and the
‘‘EXIT” sign was visible throughout the test.
3.3. Flammability test
The samples were evaluated for Flammability rating: the verti-
cal burning test as per standard UL 94-V0 and horizontal burning
test as per UL 94-HB.
As per UL standard for vertical burning test, set of five bar test
specimens (125 mm  13 mm  3 mm) were conditioned at
23 ± 2 °C and 50 ± 5% relative humidity for 48 h and five test spec-
imens were aged for 168 ± 2 h at 70 ± 2 °C and then cooled in the
desiccator for at least 4 h at room temperature [6].
The specimen is vertically mounted and flame application of
10 s is applied for twice. Depending upon the flame time after
the removal of flame source and the dripping nature of the mate-
rial, they could be classified in three categories viz. V0, V1 and
V2. Out of these three, V0 is the stringent with best fire-
retardant property. The shroud material is passed this test with
the total flame time measured to be zero second and thus, classi-
fied as UL-94 V0 rated.
As per UL standard for horizontal burning test, five test speci-
mens of dimension 125  13  3 mm were subjected to flame for
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5
30 s. As per the standard, a material classed HB shall not have a
burning rate exceeding 40 mm per minute over a 75 mm span
for specimens having a thickness of 3.0 to 13 mm [6]. This shroud
material is passed this test and classified as UL 94-HB rating as the
flame extinguishes before reaching 25 mm mark. As per UL-94 HB,
a material classified HB in the 3.0 + 0.2 mm thickness shall auto-
matically be classed HB down to a 1.5 mm minimum thickness
without additional testing.
3.4. Halogen & phosphorous test
The formulation was evaluated for halogen content as per IEC
60754-part 1, IEC 60754-part2 and DIN EN 14582. The standard
IEC 60754-1 [7] specifies a test for determination of the amount
of halogen acid gas other than the hydrofluoric acid evolved during
combustion of compound based on halogenated polymers and
compounds containing halogenated additives. The sample was
conditioned at 23 ± 2 °C and 50 ± 5% relative humidity for 24 h.
1 g of sample was then subjected to combustion at 800 °C for
20 min. The evolved gases e.g. HCl are absorbed into water inside
the chamber fed with air flow. The water is then tested with its
acidity. If the hydrochloric acid yield is less than 5 mg/g (0.5%),
the specimen is categorized as LSZH. The formulation in this work
is found to have zero percent halogen acid value and thus, complies
with the requirements of IEC 60754-1.
As per IEC 60754-2 [8], 1gm of sample was conditioned at
23 ± 2 °C and 50 ± 5% relative humidity for 16 h. The sample was
then subjected to combustion at 935 °C for 30 min. The evolved
gases were trapped to form an aqueous solution and the acidity
(pH) and conductivity of the aqueous solution was a measure of
the halogen concentration. AS per the standard, the specimen is
deemed to pass this test if the pH value is more than 4.3 and con-
ductivity is less than 10 ms/mm. The formulation in this work was
found to have pH value of 4.6 and conductivity 2.58 ms/mm and
thus complies with the requirement of IEC 60754-2.
As per DIN EN 14582 [9], the sample is oxidized by combustion
in a closed system containing oxygen (calorimetric bomb). Com-
bustion product of halogens (fluoride, chloride, bromide, iodide)
are then absorbed or dissolved in an aqueous solution. Analytical
methods like ion chromatography was used to measure the halo-
gen concentration in the absorption solution. No halogen was
detected in this sample and thus, it complies to criteria of zero
halogen fire retarding material.
3.5. Dielectric test
Dielectric Strength is a measure of the electrical strength of a
material as an insulator. Dielectric strength is defined as the max-
imum voltage required to produce a dielectric breakdown through
the material. A higher dielectric strength represents a better qual-
ity of insulator.
Dielectric Breakdown Voltage was evaluated as per ASTM D149,
Method-A [10]. The voltage was applied uniformly to the test elec-
trodes with rate of 2 kV/s rise until breakdown occurs. The average
ambient temperature was 26 ± 1 °C and relative humidity was
52 ± 1% during the test. The dielectric breakdown voltage of this
material was found to be 32.11 kV/mm and the mode of break-
down was found to be punctured at the edge of the HV Electrode.
Arc resistance is a measure of the time required to make an
insulating surface conductive under a high voltage, low current
arc in carefully controlled laboratory conditions. By this action a
conductive path is made due to thermal & chemical decomposition
and erosion. The dry arc resistance was evaluated as per ASTM
D495 [11]. The average ambient temperature and relative
humidity during the test was 26 ± 1 °C and relative humidity was
6 S. Mohapatra et al. / Materials Today: Proceedings xxx (xxxx) xxx
55 ± 1%. The dry arc resistance was found to be 270 s. Thus, the
material has good dielectric properties that is suitable for shroud.
4. Conclusion
A fire-retardant rubber composition is developed which satis-
fies the UL94-V0 and UL94-HB category. Moreover, this formula-
tion is low smoke generating as evaluated from smoke density
test with a smoke rating of less than 20%. A high limiting oxygen
index of 42.8%, ensures a good flame-retardant property along with
a temperature index of more than 250 °C. The formulation also not
found to contain any toxic halogen and phosphorous. Thus, the
developed formulation is categorized as Low smoke zero halogen
zero phosphorous (LSZHZP) and meets the criteria to suitable for
shroud with working temperature of
60 °C to +200 °C.
CRediT authorship contribution statement
Sunita Mohapatra: Conceptualization, Methodology, Writing -
original draft, Supervision. Pallabi Sarkar: Data curation, Method-
ology, Validation. Ganesh Bhoye: Software.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Please cite this article as: S. Mohapatra, P. Sarkar and G. Bhoye, A low smoke zero halogen zero phosphorous fire-retardant rubber shroud, Materials Today:
Proceedings, https://doi.org/10.1016/j.matpr.2020.04.815
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