KH C-NES 713
1.Safety Precautions
General
This test method may involve hazardous materials, operations and equipment.
Therefore, we specifically exclude any liability whatsoever for claims arising from use
or misuse of the equipment. It is the responsibility of whoever uses this equipment to
consult and establish appropriate health and safety practices and determine the
applicability of regulatory limitations prior to use.
1.
2.
The burner gases (methane and air) must be supplied, via approved regulators, with the
connections supplied and secured by approved gas hose clips.
3.
The mains power must be connected using the cable supplied by Fire Testing
Technology. Fuses must conform to Fire Testing Technology specifications.
4.
After each run it is recommended that the methane gas is turned off at the source.
5.
6.
7.
Before opening the chamber door, ensure that the excess pressure inside the chamber is
at 0 mbar. For NES 713 chambers without a pressure gauge, the pressure needs to be
equalised with the ambient. Relieve the pressure by opening the exhaust vent by pressing
the Vent button and starting the extraction fan. After 30 seconds or when the pressure is
below 5 mbar, remove the inlet vent plug. Ensure that the exhaust vent has opened by
observing the position of the shaft. Note that even a small excess pressure inside the
chamber can result in considerable force on the door, which may endanger any person
within the radius of swing of a released door.
8.
Do not lean on an open chamber door. This is because, when open, the door shifts the
centre of gravity and there may be a risk of toppling the chamber.
9.
Avoid putting fingers under the exhaust vent when open, or in the mixing fan.
10. When not in use, ensure that the door is secured ajar and that all the on/off ball valves
(Gas and Air) are closed.
FIRE FIGHTING INSTRUCTIONS: If possible, stop the flow of gas. Inerting the
atmosphere to reduce oxygen levels may extinguish flame, allowing capping of leaking
container. Do not attempt this unless specifically trained. Reduce the rate of flow and inject
an inert gas, if possible, before completely stopping the flow to prevent flashback. Do not
extinguish the fire until the supply is shut off as otherwise an explosive reignition may occur.
If the fire is extinguished and the flow of gas continues, use increased ventilation to prevent
build-up of explosive atmosphere. Use non-sparking tools to close container valves.
Use water spray to cool surrounding containers. Be cautious of a Boiling Liquid Evaporating
Vapour Explosion, BLEVE, if flame is impinging on surrounding containers. Direct 500
GPM water stream onto containers above liquid level with remote monitors. Limit the
number of personnel in proximity of fire and evacuate surrounding areas in all directions.
Firefighters should wear respiratory protection (SCBA) and full turnout or Bunker gear.
Continue to cool fire-exposed cylinders until well after flames are extinguished.
Handling and Storage
Earth ground and bond all lines and equipment associated with the system. All equipment
should be non-sparking or explosion-proof. Methane is non-corrosive and may be used with
any common structural material.
Use only in well-ventilated areas. Valve protection caps must remain in place unless
container is secured with valve outlet piped to use point. Do not drag, slide or roll cylinders.
Use a suitable hand truck for cylinder movement. Use a pressure regulator when connecting
cylinder to lower pressure piping or systems.
Do not heat cylinder by any means to increase the discharge rate of product from the
cylinder. Use a check valve or trap in the discharge line to prevent hazardous back flow into
the cylinder. Do not insert any object (i.e.: screwdriver) into valve cap openings as this can
damage the valve causing leakage.
Protect cylinders from physical damage. Store in cool, dry, well-ventilated area of noncombustible construction away from heavily trafficked areas and emergency exits. Do not
allow the temperature where cylinders are stored to exceed 125F (52C). Cylinders should
be stored upright and firmly secured to prevent falling or being knocked over. Full and empty
cylinders should be segregated. Use a "first in-first out" inventory system to prevent full
cylinders from being stored for excessive periods of time. Post "NO SMOKING signs in use
or storage areas. There should be no source for accidental ignition in areas where this product
is being used or stored. Outside or detached storage is preferred.
Do not smoke when handling methane gas.
Disposal
Waste gas should be flared through a suitable burner with a flash back arrestor. Empty
cylinders still contain flammable vapour and must be returned to the supplier.
Electrical Connection
Electrical connections between the chamber and control unit are made via a multi-core
non-reversible cable with a keyed plug and socket at each end. The mains voltage is fed into
the unit via a 3 pin socket at the rear of the Control Unit. The socket is fused into a 5 amp
fuse. The mains supply must be an earthed 110/230V A.C. (50 or 60 Hz) only, capable of
delivering at least 2 amps.
Gas Connection
Gas connections between the chamber and control unit are made via the hoses supplied, the
larger bore for the methane and the smaller bore for the air. The air and methane gas is fed
into the unit via standard gas connectors at the rear of the unit. The pressure of gas and air
going into the unit should be less than 2 bar.
It is recommended that a flame arrester is fitted externally on the combustion chamber, at the
coupling between the flexible hose and the cabinet.
Mixing Fan
A mixing fan is mounted horizontally and centrally inside the chamber at roof level and is
switched on and off externally from the Control Unit.
Specimen Support
A clamp stand holds the specimen support in place over the flame. The support is a metal
ring with temperature resistant wires (Nickel-chromium alloy wire 0.5 mm diameter)
approximately 10 mm apart to form a lattice.
10
Control Switches
These are the five red switches on the front panel. They are operated by firm pressure and
light up when activated. A detailed description of the control switches is given below:POWER
This allows the mains electrical supply through to the control unit
electronics. Once this is ON the other control switches can be operated
independently.
IGNITION
FAN
This operates the mixing fan mounted inside and at the top of the
Combustion Chamber. The fan mixes the combustion products inside
the chamber to prevent the heavier particles settling to the bottom
whilst the gases are undergoing analysis.
VENT
This opens the exhaust vent mounted in the roof of the combustion
chamber to allow removal of combustion products from the chamber
by the extraction motor.
EXTRACTION This operates the Extraction motor mounted on top of the Combustion
Chamber and extracts smoke from the chamber provided the vent is
open.
TIMER
11
Gas Analysis
For analysis of the gases the unit is supplied with a metering pump of capacity 100ml for use
with the colorimetric gas detector tubes. 1 box of each of the 14 gas detector tubes needed to
carry out the NES 713 test analysis is supplied (except for Acrylonitrile where two boxes are
provided).
Note:
In order to minimise losses of certain toxic products through adsorption, condensation, etc, prior to
measurement, all sampling lines shall be as short as possible
12
3.Test Procedure
Introduction
The Defence Standard 02-713 Issue 2 gives the requirements for one of a series of test
methods for determining the fire characteristics of materials, which are referred to in Def
Stan. 07-247.
The latest issue of the standard is available at http://www.dstan.mod.uk
The test explores the toxicity of the products of combustion in terms of a limited set of small
molecular species arising when a small specimen of a material is completely burnt under
specified conditions. A combined toxicity index is calculated from the test results using the
exposure level (in ppm) of each gas to produce fatality in 30 minutes.
The test is intended to form part of the pre-selection screening process for materials and
should not be interpreted as an assessment of toxicity hazard under actual fire conditions. The
test method is directed at the analysis of a specified set of gaseous species, which are
commonly present in combustion products of materials used in military applications and
which may cause lethality at the time of the fire. It does not address acute mental
incapacitation effects, delayed/long term toxicity, or toxicity involving particulate
combustion products. The set of gaseous species analysed is not exhaustive and the test does
not necessarily determine the total toxicity of all the constituents of the products of
combustion.
The test does not attempt to account for the influence of the rate of combustion of a material
on its contribution to toxicity hazard.
13
Specimen Preparation
Conditioning
Before cutting test specimens from the sample of material, condition the sample to a constant
mass at 23C 2C and 50% 10% relative humidity. Constant mass is considered to have
been reached when two successive weighing operations, carried out at an interval of 24 hours,
do not differ by more than 0.1 % of the mass of the sample or 0.1 g, whichever is the greater
(see BS EN ISO 291).
Specimen Size
Cut the specimens to size and store them under the same conditions until required for testing.
If the test apparatus is not located in a humidity conditioned laboratory, the test procedure
shall be started within 3 minutes after the removal of each test specimen from the
conditioning enclosure.
The size and shape of all test specimens shall be such that they are entirely engulfed in the
flame during the test.
Where possible, the test specimens shall be cut as a single piece, approximately in the form of
a cube.
Note:
Each of the test specimens for a material must be of the same size and shape.
Where the sample is a multi-layered sheet, the specimens shall be cut as a cross-section
through the full thickness of the sheet, to include a representative proportion of all
components/layers of the product.
Once the specimens have been cut from the sample of material, ensure they are handled
carefully to avoid contamination.
Specimen Mass
Unless otherwise specified, all test specimens shall have a mass of 1.000
0.050
0.000
gram.
Specimen masses other than 1 gram may be used if specified by the technical authority
named in the tender or contract in which this Def Stan. is specified, or by any relevant
material specification.
For low density materials (e.g. foams) for which a 1 gram test specimen would be too large to
be engulfed in the burner flame, then reduce the size/mass of specimens, to ensure that this
can be achieved. Use the largest possible specimens that will allow this requirement to be
met.
Also, if any of the gases give an indication that exceeds the maximum scale reading on the
colorimetric tube for that gas, then it is permissible to reduce the size/mass of specimens in
order to achieve a reading within the available maximum range. When this is necessary,
discard all of the results obtained using the original (higher mass) specimens and carry out all
of the determinations (including the measurement of all gases) in the same runs, using this
reduced specimen mass.
14
If specimens of the size determined above are found to burn for longer than 2 minutes or if
pressure in the chamber exceeds 50 mbar (whichever occurs first), then pressure inside the
chamber can become unsafe. In such cases, stop testing at 2 minutes, and do not conduct
gas analysis. Evacuate the chamber and repeat the test with a smaller specimen size/mass, to
ensure that they are completely consumed in less than 2 minutes and the pressure in the
chamber stays below 50 mbar.
FTT recommends that tests are performed without colorimetric tubes to determine the
specimen mass required to achieve all of the above criteria before conducting the full toxicity
analysis. This may mean reducing the sample size until the above criteria are met.
If any dripping or spitting of the sample occurs during the test, then glass wool or wire shall
be used to support the specimen. See 10 of Section 3.5.
Number Of Test Specimens
A minimum of two test specimens are required in order to obtain at least two determinations
for each gas.
2)
Position the burner in the centre of the test chamber floor, without the specimen support
in place. The chamber door will need to be open during this procedure.
3)
Turn on the air by using the On/Off valve and adjust the flow rate to 10-15 l/min
4)
Ensure that the Fan, Vent and Extraction buttons are off and that the Power button is On.
5)
Open the Methane On/Off valve and then press the Ignition button. Adjust the maehtane
gas flow as required to allow the burner to ignite.
6)
Adjust the flow rates of gas and air to achieve a non-luminous (blue) flame 100 mm to
125 mm in height (measured to the tip of the outer blue cone), having a temperature of
1150C 25C at its hottest point, measured with a thermocouple.
7)
Record the flame temperature, T(C), at its hottest point and note the position of this
hottest point (distance from the floor of the chamber). Also record the flow rates of the
gases.
8)
Close the chamber door and tighten the clamps. Firmly put the inlet vent plug into the
lower left side of the chamber.
9)
Press the Vent button to close the exhaust vent and check that the flame temperature is
still within 1150C 25C. If not then repeat steps 6 9.
15
Within 2 minutes or 50 mbar of chamber pressure, extract the chamber by pressing the
vent and extraction buttons.
10) Press the Ignition button and turn the two On/Off valves to the Off position to extinguish
the burner.
Note: It is best to use the clamp stand to hold the thermocouple in the flame. In this way the burner can be
moved away in order to measure the height from the chamber floor to the thermocouple.
Specimen Test
1)
Ensure that the apparatus is clear of combustion products from any previous test.
Between test runs, clean the specimen support to ensure that no residue remains. Also
clean the interior walls of the test chamber and all apparatus inside the chamber, as
necessary to remove any sooty deposits.
Note: This is important to avoid cross contamination between different specimens/materials and to prevent
the build up of sooty deposits on the inside of the chamber, which may absorb gaseous combustion
products.
WARNING
Even after venting, when the apparatus is apparently clear of combustion products,
the contaminants remaining inside the chamber may be hazardous (e.g. respiratory,
skin, eye). Note also that the apparatus may still be hot (e.g. burner and support
frame). Appropriate protection measures shall be taken to prevent exposure of the
operator.
2)
3)
Select a test specimen and determine its mass in grams to 3 decimal places.
4)
Place the test specimen on the support, approximately in the centre of the test chamber
floor. Adjust the position of the support so that the specimen will be sited within the
flame boundary at the hottest point established in Section 3.4 so it will be subjected to
the a flame temperature of 1150C 25C.
For materials that would otherwise melt and/or drip, test specimens may be supported on
a thin bed (single layer, approximately 0.02 g) of glass wool, placed on the wire mesh
support to prevent losses during the burn. The use of glass wool shall be stated in the test
report. Use a fresh piece of glass wool for each specimen.
For low density materials (e.g. foams) that are liable to be displaced/blown by the force
of the gas flame, it is permissible to hold the specimen in place on the support using a
loop of wire (for example Nickel-chromium alloy wire, 0.5 - 0.6 mm in diameter). In
doing so, do not crush or otherwise distort the test specimen. The type of wire used shall
be stated in the test report.
16
5)
Prepare the colorimetric gas reaction tubes by breaking off the end sealing parts, for the
gases to be measured, and connect each tube to a separate gas sampling port INSIDE the
chamber. Use a new short length of silicone tubing to connect the tube to the sampling
port and observe the direction of flow on the colorimetric tubes.
Each sampling port that has a colorimetric tube connected to it must be blanked off on
the outside of the chamber by tying off a short length of silicone tubing (as shown in
Figure 3.1)
Any ports not used must be sealed by either linking adjacent ports with a loop of silicone
tubing, or by tying off a length of silicone tubing. As an example the photo in Figure 3.1
shows the chamber prepared with 10 out of the 12 ports being used and the top right port
with a tied off length of silicone. The two ports linked together in the photo are not being
used.
Ensure that the Fan, Vent, Extraction and Ignition buttons are off and then close the test
chamber door and tighten the clamps. Then firmly insert the inlet vent plug in the lower
side of the chamber.
7)
Then turn on the air On/Off valve. (Note that the exhaust vent is still open)
8)
To start the test, turn on the gas On/Off valve, press the Ignition button and the Vent
button simultaneously and start the timing device.
WARNING
For safety reasons, if the burner does not ignite within a few seconds, turn off the gas
and air supplies and evacuate the chamber (push Vent Off and push Extraction On).
This is to avoid the build up of un-ignited gas in the chamber. Re-adjust the burner
settings to achieve ignition and carry out a repeat test.
17
9)
Throughout the test, make observations of the behaviour of the specimen and note the
times at which the observations were made, including whether or not the specimen
ignites, plus other behaviour such as charring, melting, dripping, shrinkage,
intumescence, fragmentation, explosive decomposition/spitting, erratic burning, afterglow, or any loss of material from the specimen.
10) If any material is lost from the specimen during the test (e.g. by dripping or spitting) or
the specimen moves, so that any part is no longer within flame boundary, then the test
shall be halted and the results discarded. A repeat test shall be carried out with a fresh
specimen, using glass wool or wire to support the specimen.
11) The duration of the burn is to be sufficient to ensure that all of the combustible material
within the specimen is completely consumed.
During a test run, while gas and air are being fed to the burner, there is likely to be an
increase in the pressure inside the test chamber because it is sealed. It is important not to
continue to run the burner for longer than 2 minutes or exceed 50 mbar of pressure, as
this pressure build up may cause the chamber to leak and/or may be dangerous. It is
therefore important not to use oversize test specimens (see Section 3.3.3), which may
take longer to be completely burnt.
Note: Even for the same material, from specimen to specimen there may be small variations in the time taken
for combustion to be complete. It is therefore recommended in the first run, to continue the burn after
all signs of combustion of the specimen have ceased, up to the next increment of 15 seconds, to allow
for the possibility that subsequent specimens may burn for slightly longer. Typical burn times are
therefore 60 s, 75 s, 90 s.
12) When the burn is judged complete, extinguish the burner by turning the methane and air
On/Off valves Off and push the Ignition button. Record the time as the burn time, tburn
(seconds). The same burn time shall be used for each of the subsequent specimens tested
for the same material.
Note: If the material does not ignite or show any other signs of production of gases from the specimen in the
first 60 seconds of the burn, stop the run at 60 seconds, as described above and continue the procedure
using this as the burn time (i.e. t = 60 seconds). This behaviour shall be recorded in the test report.
13) Immediately start the mixing fan (push the Fan button On) and continue mixing for 30
seconds, then switch off the fan (push the Fan button Off).
14) Then immediately commence sampling the atmosphere from the chamber by drawing
the gas mixture through the sampling ports using the supplied metering pump. Use a
short length of silicone tubing to connect the sampling port to the metering pump. Some
notes on the use of colorimetric tubes are given in Section 3.7.
Analysis for halide gases must be carried out first, in order to minimise potential losses
through adsorption, condensation, etc, which may be experienced through a delayed
estimation.
18
The room exhaust system must be switched on and connected to the outlet of the extraction pump on
the instrument.
16) After 30 seconds or when the chamber pressure is below 5 mbar, remove the inlet vent
plug from the lower left side of the chamber.
17) When all the smoke is removed from the chamber then open the chamber door, replace
the inlet vent plug and push the Extraction button Off.
WARNING
Even after venting, when the apparatus is apparently clear of combustion products,
the contaminants remaining inside the chamber may be hazardous (e.g. respiratory,
skin, eye). Note also that the apparatus may still be hot (e.g. burner and support
frame). Appropriate protection measures shall be taken to prevent exposure of the
operator.
18) Examine the residue of the test specimen to ensure that all of the combustible material
has been consumed. If any portion of the combustible material remains unburnt or
appears to be, discard the results and carry out a repeat test run using a fresh specimen
and a longer burn time (or if necessary using a smaller specimen).
19) After the first specimen burn, carry out a determination of the background (burner)
corrections (see Section 3.6).
20) Repeat steps 1) to 18), with fresh specimens, using the same burn time and specimen
form, for as many times as necessary to obtain at least two consistent determinations for
each gas.
19
Note:
It may be necessary to reduce the specimen mass if gas concentrations exceed the measurement range
of the colorimetric tubes.
21) After the last specimen burn carry out a further determination of the background (burner)
corrections (see Section 3.6).
22) The whole procedure can then be repeated for the next sample.
2)
With the cleaned specimen support in place, but no specimen in the chamber, place
carbon monoxide, carbon dioxide and nitrous oxides colorimetric tubes in position. Use
a new short length of silicone tubing to connect the tube to the sampling port and
observe the direction of flow on the colorimetric tubes. Ensure that all other sampling
positions are sealed. Seal all used ports with a tied off short length of silicone tubing.
3)
Ensure that the Fan, Vent, Extraction and Ignition buttons are off and then close the test
chamber door and tighten the clamps. Then firmly insert the inlet vent plug in the lower
left side of the chamber.
4)
Then turn on the air On/Off valve. (Note that the exhaust vent is still open)
5)
To start the test, turn on the gas On/Off valve, press the Ignition button and the Vent
button simultaneously and start the timing device.
WARNING
For safety reasons, if the burner does not ignite within a few seconds, turn off the gas
and air supplies and evacuate the chamber (push Vent Off and push Extraction On).
This is to avoid the build up of un-ignited gas in the chamber. Re-adjust the burner
settings to achieve ignition and carry out a repeat test.
20
6)
After tburn seconds extinguish the burner by turning the methane and air On/Off valves
Off and push the Ignition button.
7)
Immediately start the mixing fan (push the Fan button On) and continue mixing for 30
seconds, then switch off the fan (push the Fan button Off).
8)
Then immediately commence sampling the atmosphere from the chamber by drawing
the gas mixture through the sampling ports using the supplied metering pump to
determine the concentrations of carbon monoxide, carbon dioxide and nitrous oxides.
Use a short length of silicone tubing to connect the sampling port to the metering pump.
9)
On completion of the analysis, clear the remaining products of combustion from the
chamber push the Vent button Off, then the Extraction button On.
Note:
The room exhaust system must be switched on and connected to the outlet of the extraction pump on
the instrument.
10) After 30 seconds or when the chamber pressure is below 5 mbar, remove the inlet vent
plug from the lower left side of the chamber.
21
22
Tube reading = 0
Ci(HBr) = 0
Ci(HCl) = 0
Lassaigne
analysis of sample
Negative for Br
Positive for Br
23
Subtract the respective background (burner) corrections, determined in Section 3.6, from
the carbon monoxide, carbon dioxide and nitrous oxides concentrations measured in the
chamber for each test run to give the actual values resulting from combustion of the test
specimen.
2)
For each determination, use the equation given below to calculate (in ppm) the
concentration of the gas, produced under the conditions of the test, scaled up for 100
grams of material and re-calculated as though the combustion products were diffused
into a volume of 1 m3 using equation (1):
Ci
(1)
100 V
8
where,
Ci = concentration of gas i in test chamber, resulting from combustion of the test specimen
(ppm)
m = mass of test specimen (g)
V = volume of test chamber (m3)
3)
4)
C81
C f1
C8 2
C f2
C8 3
C f3
C8n
(2)
C fn
where,
1, 2, 3,,n represent each of the n gases detected;
C 8 i = the average value of C 8 for the gas i calculated in step 3) above (ppm);
C f = concentration of the gas i considered fatal to man for a 30 minute exposure time
i
Values of Cf are given in Table 3.1 (ppm).
24
Gas
Cf (ppm)
100 000
4000
750
Ammonia (NH3)
750
Formaldehyde (HCHO)
500
500
Acrylonitrile (CH2CHCN)
400
400
250
Phenol (C6H5OH)
250
150
150
100
Test Report
The test report shall include a reference to Def Stan 02-713 Issue 2, together with the
following information:
a) the name and address of the laboratory undertaking the test;
b) the name and address of the supplier and where different, of the manufacturer of the
material tested and the sponsor of the test;
c) the date(s) of the test;
d) a full description of the material tested, including;
commercial name, including any unique identification number or grade reference
batch number
laboratory sample reference number/code
NATO stock code no.
material or product specifications to which the material complies (e.g. Def Stan.
BS, etc)
application (e.g. deck covering, thermal insulation, etc)
material type (i.e. generic description of the chemical nature or composition e.g.
wood, EPDM rubber, mineral wool, etc)
type of product (i.e. form or shape e.g. sheet, pipe/tube, coating, foam, moulded
shape, fabric, etc)
essential dimensions (e.g. mass or density, sheet size/thickness, layers, etc.)
colour (in the case of paints/coatings the finish coat surface colour)
25
coatings details (e.g. temporary substrate used to produce free films, application
method (brush/spray), no. of layers, coverage rates, thicknesses, etc.)
details of any previous test known
other relevant information about the sample, useful in identifying the material
tested
e) a full description of the specimens tested, including approximate shape and
dimensions and the location and orientation from which the specimens were taken in
relation to the sample and any inhomogeneity of the material (e.g. surfaces, edges,
layers, machine directions, multiple phases, etc);
f) whether the specimen was supported on glass wool or held with wire and type of wire
used;
g) the analytical method and the calibrated measurement range, used for each gas;
h) the volume of the test chamber, V;
i) the burn time, tburn;
j) the flame temperature, T and gas used (i.e. methane or natural gas);
k) the individual and average values for the background corrections for carbon monoxide
(CO), carbon dioxide (CO2) and nitrous oxides (NOx);
l) for each valid determination, values of m, Ci, C8
m) for each gas detected, the average value of C8 and C8 Cf ;
n) the Toxicity Index (TI) of the material (per 100g) rounded to 1 decimal place;
o) observations of the burning behaviour of the specimens and the times at which the
observations were made, together with reasons for any invalid tests;
p) a note of any possible cross reactions of the colorimetric gas reaction tubes;
q) a note of any deviations from the standard protocol, such as the use of reduced size
specimens;
r) the statement: "This test result alone does not assess the fire hazard of the material, or
a product made from this material, under actual fire conditions. Consequently, the
results of this test alone are not to be quoted in support of claims with respect to the
fire hazard of the material or product under actual fire conditions.
26
NOTES
Should any errors or omissions be found in this users guide or should you require any further
information, please contact Fire Testing Technology Limited. Telephone: +44 (0)1342
323600 or Fax: +44 (0)1342 323608.
27
28
Appendix A:
The spare parts list for the NES 713 Apparatus is given in the following pages. Please contact
FTT or their agents if there are any spares items not included on the list that you require or for
prices.
29
30