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Tiêu đề Toxicity of Fire Effluent — Summary and Relevance of Test Methods
Trường học British Standards Institution
Chuyên ngành Fire Hazard Testing
Thể loại Standard
Năm xuất bản 2011
Thành phố Brussels
Định dạng
Số trang 52
Dung lượng 1,33 MB

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Cấu trúc

  • 4.1 General (18)
  • 4.2 Toxic potency (18)
  • 4.3 Fractional effective dose (FED) and toxic hazard (19)
  • 4.4 Fractional effective concentration (FEC) (20)
  • 4.5 Generic toxic potencies (20)
  • 5.1 General (20)
  • 5.2 Physical fire models (20)
  • 5.3 Fire stages in a compartment fire (23)
  • 5.4 Methods of analysis (23)
    • 5.4.1 Chemical analysis based methods (24)
    • 5.4.2 Methods based on animal exposure (24)
  • 6.1 General (24)
  • 6.2 UK Ministry of Defence – Defence Standard (DS) (25)
    • 6.2.1 Summary (25)
    • 6.2.2 Purpose and principle (25)
    • 6.2.3 Test specimen (25)
    • 6.2.4 Test method (25)
    • 6.2.5 Repeatability and reproducibility (26)
    • 6.2.6 Relevance of test data and special observations (26)
    • 6.2.7 Reference document (27)
  • 6.3 Airbus industry (27)
    • 6.3.1 Summary (27)
    • 6.3.2 Purpose and principle (27)
    • 6.3.3 Test specimen (27)
    • 6.3.4 Test method (27)
    • 6.3.5 Repeatability and reproducibility (28)
    • 6.3.6 Relevance of test data and special observations (28)
    • 6.3.7 Reference documents (28)
  • 6.4 Comitato Elettrotecnico Italiano (CEI) (28)
    • 6.4.1 Summary (28)
    • 6.4.2 Purpose and principle (28)
    • 6.4.3 Test specimen (28)
    • 6.4.4 Test method (28)
    • 6.4.5 Repeatability and reproducibility (28)
    • 6.4.6 Relevance of test data and special observations (29)
    • 6.4.7 Reference documents (29)
  • 6.5 Norme Franỗaise (NF) (29)
    • 6.5.1 Summary (29)
    • 6.5.2 Purpose and principle (29)
    • 6.5.3 Test specimen (29)
    • 6.5.4 Test method (29)
    • 6.5.5 Repeatability and reproducibility (30)
    • 6.5.6 Relevance of test data and special observations (30)
    • 6.5.7 Reference documents (30)
  • 6.6 International Electrotechnical Commission (IEC) (30)
    • 6.6.1 Summary (30)
    • 6.6.2 Purpose and principle (30)
    • 6.6.3 Test specimen (31)
    • 6.6.4 Test method (31)
    • 6.6.5 Sampling of effluent (31)
    • 6.6.6 Repeatability and reproducibility (32)
    • 6.6.7 Relevance of test data and special observations (32)
    • 6.6.8 Reference documents (32)
  • 6.7 International Standards Organization (ISO) (32)
    • 6.7.1 Summary (32)
    • 6.7.2 Purpose and principle (32)
    • 6.7.3 Test specimen (32)
    • 6.7.4 Test method (32)
    • 6.7.5 Repeatability and reproducibility (33)
    • 6.7.6 Relevance of test data and special observations (33)
    • 6.7.7 Reference documents (33)
  • 6.8 International Maritime Organization (IMO) (33)
    • 6.8.1 Summary (33)
    • 6.8.2 Purpose and principle (33)
    • 6.8.3 Test specimen (33)
    • 6.8.4 Test method (33)
    • 6.8.5 Repeatability and reproducibility (34)
    • 6.8.6 Relevance of test data and special observations (34)
    • 6.8.7 Reference documents (34)
  • 6.9 Toxicity test for rolling stock cables (34)
    • 6.9.1 Summary (34)
    • 6.9.2 Purpose and principle (35)
    • 6.9.3 Test specimen (35)
    • 6.9.4 Test method (35)
    • 6.9.5 Repeatability and reproducibility (36)
    • 6.9.6 Relevance of test data and special observations (36)
    • 6.9.7 Reference document (36)
  • 7.1 Deutsches Institut für Normung (DIN) (36)
    • 7.1.1 Summary (36)
    • 7.1.2 Purpose and principle (37)
    • 7.1.3 Test specimen (37)
    • 7.1.4 Test method (37)
    • 7.1.5 Repeatability and reproducibility (37)
    • 7.1.6 Relevance of test data and special observations (37)
    • 7.1.7 Reference documents (38)
  • 7.2 National Bureau of Standards (NBS) (38)
    • 7.2.1 Summary (38)
    • 7.2.2 Purpose and principle (38)
    • 7.2.3 Test specimen (38)
    • 7.2.4 Test method (38)
    • 7.2.5 Repeatability and reproducibility (39)
    • 7.2.6 Relevance of test data and special observations (39)
    • 7.2.7 Reference documents (39)
  • 7.3 National Institute of Standards and Technology (NIST) (39)
    • 7.3.1 Summary (39)
    • 7.3.2 Purpose and principle (40)
    • 7.3.3 Test specimen (40)
    • 7.3.4 Test method (40)
    • 7.3.5 Repeatability and reproducibility (41)
    • 7.3.6 Relevance of test data and special observations (41)
    • 7.3.7 Reference documents (41)
  • 7.4 University of Pittsburgh (Upitt) (41)
    • 7.4.1 Summary (41)
    • 7.4.2 Purpose and principle (41)
    • 7.4.3 Test specimen (41)
    • 7.4.4 Test method (42)
    • 7.4.5 Repeatability and reproducibility (42)
    • 7.4.6 Relevance of test data and special observations (42)
    • 7.4.7 Reference documents (42)
  • 7.5 Japanese fire toxicity test for building components (43)
    • 7.5.1 Summary (43)
    • 7.5.2 Purpose and principle (43)
    • 7.5.3 Test specimen (43)
    • 7.5.4 Test method (43)
    • 7.5.5 Repeatability and reproducibility (43)
    • 7.5.6 Relevance of test data and special observations (43)
    • 7.5.7 Reference documents (44)

Nội dung

IEC 60695-7-1 2010 Fire hazard testing - Part 7-1: Toxicity of fire effluent - General guidance EN 60695-7-1 2010 IEC/TS 60695-7-3 - Fire hazard testing - Part 7-3: Toxicity of fire ef

General

Small-scale toxicity tests, especially toxic potency tests, are essential for producing data utilized in toxic hazard assessments, fire hazard evaluations, and fire-safety engineering calculations.

Many tests are mistakenly viewed as directly indicating the toxicity or toxic hazard of a material or product This misinterpretation contradicts the guidance provided in ISO 19706 and IEC 60695-7-1, potentially resulting in false assumptions regarding the toxic hazard contributions of specific materials or products.

Therefore, the data from small-scale toxicity tests should not be used directly in product specifications, or to imply in isolation, any level of toxic hazard

Data from toxic potency test methods should be utilized as a component of a comprehensive toxic hazard assessment This should be done alongside other fire-related product data, including mass loss rate.

Toxic potency

Toxic potency is a key concept in fire science, referring to the amount of a toxicant needed to produce a specific toxic effect A widely recognized measure of toxic potency is the LCt50, which indicates the lethal exposure dose required to cause the death of 50% of the organisms exposed.

The exposure dose of the i th toxic component, [ ] D i , in a mixture of toxic components, is defined by the following equation:

D = ∫ = 1 ∫ = or, if the volume fraction of the i th toxic component is constant over time,

C i is the volume fraction of the i th toxic component;

X i is the volume yield of the i th toxic component from a toxic potency test;

The mass loss concentration integral, denoted as D m, represents the total mass lost during the exposure time, t, divided by the volume of the fire effluent Here, m refers to the mass of the test specimen that is lost throughout the exposure duration.

V is the volume into which the fire effluent is dispersed

In both cases the exposure dose has units of volume fraction × time, e.g min

In some cases, m/V, known as "mass loss concentration", is used instead of the volume fraction, in which case the exposure dose has units of concentration × time, e.g g × min × m -3

A 30-minute exposure to a mass loss concentration of 20 g × m⁻³ results in a toxic potency of 600 g × min × m⁻³ This indicates that a 10-minute exposure to a concentration of 60 g × m⁻³ is expected to produce the same defined effect Additionally, a 20-minute exposure to a higher mass loss concentration would similarly lead to the defined effect.

30 g × m -3 is also assumed to cause the same defined effect

The toxicity of fire effluent from materials depends on the physical fire model employed, with temperature and ventilation conditions being crucial factors Further details are provided in section 5.1.

Fractional effective dose (FED) and toxic hazard

Toxic potency is a key factor in assessing the toxic hazard of fire scenarios, as it indicates the toxic effects of fire effluent per unit of mass loss To accurately estimate the toxic hazard of a specific product, it is crucial to understand both the amount of fire effluent released over time and the volume into which this effluent disperses.

The toxic hazard of a material is determined by the product of its toxic potency and the mass loss rate Consequently, a substance with high toxic potency and a low mass loss rate can present a similar toxic hazard as one with low toxic potency and a high mass loss rate.

Fractional effective concentration (FEC)

To assess the toxic hazard of sensory and upper respiratory irritants, the primary focus is on the concentration of each irritant Fractional effective concentrations (FECs) are calculated for each irritant over specific time intervals The cumulative FECs must not exceed a predetermined threshold value, which indicates the available time for safe escape according to established safety criteria (refer to ISO 13571).

Generic toxic potencies

To conduct a toxic hazard assessment, it is not always essential to possess toxic potency data for the materials involved Research from ISO and other publications indicates that most materials generate fire atmospheres with comparable toxic potency.

For an initial toxic hazard assessment in fire scenarios, it is advisable to use a generic toxic potency of 900 g × min × m^{-3} for well-ventilated pre-flashover fires and 450 g × min × m^{-3} for vitiated post-flashover fires, as outlined in ISO 13571:2007 To evaluate the reliability of this assumption, the assessment should be repeated using toxic potency values at 50% and 200% of the generic value If these alternative values significantly alter the assessment results, more precise toxic potency data may be necessary.

5 General aspects of small-scale toxicity tests

General

Small-scale toxicity tests consist of two main components: first, the decomposition conditions, which involve a physical fire model that generates fire effluent with a composition similar to that produced during specific stages of a real fire Second, the evaluation methods assess the toxic potency of the fire effluent, either by exposing animals in a controlled environment to monitor their responses or by conducting chemical analyses to estimate toxic potency based on the concentrations of various substances.

A critical part of any method is to be able to relate the toxic effect or concentrations observed to the mass loss of the material under test.

Physical fire models

A given material does not have a single toxic potency associated with it

The composition of fire effluent from a material is not an intrinsic property but is significantly influenced by the burning conditions Consequently, the toxic potency of fire effluent varies based on these conditions Key factors such as decomposition temperature and ventilation levels play a crucial role in determining the composition of fire effluent and its associated toxicity.

The presence of certain variables significantly influences the types and quantities of asphyxiant and irritant species generated For instance, materials containing nitrogen can lead to the formation of ammonia and hydrogen cyanide under vitiated conditions, while well-ventilated environments typically result in the production of nitrogen oxides.

Burning conditions significantly influence the efficiency of carbon conversion into carbon oxides, specifically carbon monoxide and carbon dioxide A reduced CO 2 /CO ratio signifies a higher concentration of carbon monoxide, leading to an increased toxic potency value, indicating greater toxicity.

Demonstrating the relevance of test conditions in a standardized physical fire model to the specific fire scenario is essential ISO 19706 provides a general classification of fire types, as illustrated in Table 1 Key factors influencing the toxic potency of fire effluent include oxygen concentration and irradiance/temperature.

ISO 16312-1 provides criteria for assessing the validity of physical fire models used to obtain fire effluent toxicity data for fire hazard and risk assessment Additionally, ISO/TR 16312-2 evaluates individual physical fire models.

ISO 19703 outlines the definitions and equations necessary for calculating toxic product yields, detailing the fire conditions associated with these calculations in relation to equivalence ratio and combustion efficiency.

Table 1 – Characteristics of fire types (ISO19706) Fi re t yp e He at f lu x to fu el s ur fa ce kW /m 2

Ma x t em pe ra tu re ° C Ox yg en vo lu m e % Fue l/a ir eq ui val en ce ra ti o (p lu m e) ] [C O [C O ] 2 v/ v

The efficiency of fuel surfaces in various combustion scenarios is influenced by several factors In non-flaming conditions, self-sustaining processes are not applicable, while oxidative pyrolysis occurs at temperatures between 300 to 600°C Anaerobic pyrolysis, also influenced by external radiation, operates at lower temperatures of 100 to 500°C Well-ventilated flaming conditions exhibit oxygen consumption ratios less than 1, with temperatures ranging from 350 to 650°C In under-ventilated flaming scenarios, localized fires can reach temperatures of 300 to 600°C, with oxygen demands exceeding 1 The upper layer temperature is primarily determined by the source of externally applied radiation and room geometry The combustion rate is controlled by fuel availability, and the equivalence ratio can significantly vary based on material chemistry and local conditions.

Fire stages in a compartment fire

A general pattern can be established for fire development within a compartment, where the general temperature-time curve shows three stages, plus a decay stage (see Figure 1 and Table 1)

Stage 1, known as non-flaming decomposition, marks the initial phase of a fire before sustained flaming occurs, characterized by minimal temperature rise and significant threats from smoke and toxic emissions During this stage, fire types 1a, 1b, and 1c may manifest Stage 2, or the developing fire phase, begins with ignition and is defined by a rapid increase in room temperature, alongside the spread of flames, heat release, and further production of smoke and toxic effluents, corresponding to fire type 2 Finally, Stage 3, the fully developed fire stage, occurs when all combustible materials in the room have decomposed sufficiently, leading to a sudden ignition throughout the space, resulting in a dramatic temperature surge known as flashover, which aligns with fire type 3b.

At the conclusion of Stage 3, the combustibles and oxygen are mostly depleted, leading to a decrease in temperature This decline occurs at a rate influenced by the system's ventilation and its heat and mass transfer properties, a phase referred to as the decay stage.

In each of these stages, a different mixture of decomposition products may be formed and this, in turn, will influence the toxicity of the fire effluent produced during that stage

Fully developed fire Decay stage

C om par tm ent te m per at ur e

Figure 1 – Different phases in the development of a fire within a compartment

Methods of analysis

Chemical analysis based methods

Chemical analysis methods employ traditional laboratory techniques to measure the concentrations of different gases in the fire effluent produced by physical fire models, either in a static or dynamic manner.

The accuracy of chemical analysis techniques is significantly influenced by various factors, particularly the selection of effluent species for analysis It is essential to choose a diverse range of species that adequately represents those likely to be released, informed by an understanding of the material's composition being tested.

It is essential to measure carbon dioxide, carbon monoxide, and oxygen levels during testing A reliable method must be in place to assess the mass loss of the test specimen, enabling the conversion of measured gas concentrations to values per unit mass loss Additionally, the conversion of these gas concentrations and mass loss into toxic potency values is necessary, as outlined in IEC 60695-7-3.

In ISO 19701, methods for the sampling and analysis of fire effluents are reviewed, and in ISO 19702 guidance is given on the use of FTIR (Fourier transform infra-red analysis).

Methods based on animal exposure

It is not recommended that any further work should be conducted on methods based on animal testing

NOTE If test specimen mass loss is not measured in an animal exposure test, then the yields of toxic components cannot be calculated

6 Summary of published chemical analysis based test methods

General

This summary does not replace published standards, which are the only valid reference documents

This section reviews chemical analysis-based test methods that are recognized as international, national, or industry standards commonly used in the electrotechnical field It does not aim to cover all available test methods.

1 Numbers in square brackets refer to the bibliography.

UK Ministry of Defence – Defence Standard (DS)

Summary

The DS 02-713 test evaluates the toxicity of combustion products by analyzing small molecular species generated when a material sample is fully combusted in excess air under controlled conditions.

Purpose and principle

The analytical data of small molecular gaseous species produced from the complete combustion of the tested material under flaming conditions are mathematically analyzed This analysis uses the exposure level (volume fraction) of each gas that can lead to death within 30 minutes as a foundation to calculate a combined toxicity index.

Test specimen

To ensure optimal analytical precision, a minimum of three test specimens are prepared from the material being tested The mass of each specimen is carefully selected based on the characteristics of the combustion products and the sensitivity of the analytical method used.

Test method

The apparatus consists of an airtight chamber with a minimum volume of 0.7 m³, lined with opaque polypropylene sheeting It features a mixing fan and utilizes a methane Bunsen burner as the heat source, operating at a temperature of 1,150 °C ± 50 °C The test specimen is positioned within the flame boundary to ensure complete combustion, and the duration of the burn period is meticulously recorded.

The atmosphere in the test chamber is analyzed using colorimetric gas detection tubes After the burner is extinguished following complete combustion, a mixing fan operates for 30 seconds before being turned off to allow for gas sampling Initial tests focus on halogen-containing gases, with the monitored gases including carbon monoxide, carbon dioxide, hydrogen sulfide, ammonia, formaldehyde, hydrogen chloride, acrylonitrile, sulfur dioxide, nitrogen oxides (NO x), phenol, hydrogen cyanide, hydrogen bromide, hydrogen fluoride, and phosgene.

A background correction factor for the gases to be measured is also determined using a test run with no sample present

The results are expressed as a toxicity index, based on a weighted calculation as follows:

C f is the volume fraction of the gas considered lethal for a 30 min exposure time as shown in Table 2;

C θ is the volume fraction of each gas produced when 100 g of material is burnt and the combustion products are dispersed into 1 m 3 of air

Table 2 – C f values taken from DS 02-713 for various gases

Repeatability and reproducibility

Early test versions exhibited low reproducibility due to insufficient specifications of the test chamber Additionally, the reliance on colorimetric tubes led to considerable errors, stemming from both the tubes' imprecision and the time lag associated with the sequential analysis method Notably, gas concentrations can significantly decay during the sampling period, which may extend up to 30 minutes.

Relevance of test data and special observations

The current test method faces significant criticism due to several factors: a) the flame temperature and ventilation conditions result in a physical fire model that does not align with any fire types listed in Table 1; b) the outdated weighting values in the overall toxicity index calculation may introduce unjustified bias against specific material classes; and c) the data presentation is inappropriate for toxic hazard assessment.

This method is not advisable for the development of electrotechnical products and should not serve as a foundation for regulations or controls regarding toxic hazards Due to the limitations of the physical fire model, calculation methods, and data format, the results from this test are unsuitable for toxic hazard assessments, fire hazard evaluations, or fire safety engineering calculations.

Many physical fire models do not specify the combustion rate, allowing flame-retarded materials to burn at the same rate as non-retarded materials Consequently, for accurate fire hazard assessments, it is essential to gather additional data on combustion rates across various fire types.

This test method is discussed in ISO 16312-2

The UK Ministry of Defence intends to replace this test with NATO AFAP-3 (see 6.4.6).

Reference document

Airbus industry

Summary

Airbus ABD 0031 outlines the fireworthiness design criteria for the pressurized sections of Airbus commercial aircraft, detailing the fire-smoke-toxicity (FST) requirements and relevant testing methods This document specifically addresses the toxicity requirements essential for ensuring passenger safety.

Purpose and principle

Non-metallic components and sub-assemblies designed for use within the pressurized section of transport category aircraft must undergo testing as outlined in section 6.3.4, excluding small parts like knobs, handles, rollers, fasteners, clips, grommets, rubber strips, pulleys, and minor electrical components.

Test specimen

The test method uses the same size test specimens as described in IEC 60695-6-30 [5], i.e 76,2 mm × 76,2 mm × the intended installation thickness.

Test method

The test is performed in combination with (not simultaneously) the smoke density test in the NBS (National Bureau of Standards) smoke chamber according to ASTM E-662 [6]

The gas sampling procedure starts immediately after the 4 min smoke test run and after

16 min for electrical wire/cable insulation materials

At least two test specimens are tested for each test condition (flaming and non-flaming)

Chemical analysis methods, such as ion chromatography and gas chromatography, are commonly employed Alternative methods can be utilized, provided that comparison tests demonstrate they yield equivalent results.

The volume fractions of specific gases are evaluated against established specification limits It is crucial that the average volume fraction of these smoke gas components remains within the limits specified in Table 3 during the relevant test durations of 4 minutes and 16 minutes, applicable to both flaming and non-flaming conditions.

Table 3 – Volume fraction limits for gas components

Gas component Limit of volume fraction × 10 6

Repeatability and reproducibility

Relevance of test data and special observations

Fire and ventilation conditions do not allow a comparison between this physical fire model and any of the fire types described in Table 1

Only a limited number of gas components is considered.

Reference documents

Comitato Elettrotecnico Italiano (CEI)

Summary

The CEI 20-37/7 test is utilized to assess the opacity and corrosivity of smoke, as well as to determine the toxicity index of gases released during the combustion of electric cables and their materials.

Purpose and principle

This test is used to measure the quantity of various gases evolved during the combustion of a small test specimen of material in a tube furnace with continuous air flow

A toxicity index is calculated based on measured gas concentrations and a series of weighting factors.

Test specimen

The test specimen, with a typical mass of 1,0 g, consists of a piece of material or a test specimen cut from an end-product.

Test method

The test specimen is introduced into a quartz tube in a tube furnace set at 800 °C ± 10 °C and an air flow of 120 l × h –1 ± 5 l × h –1 is passed through the tube and over the test specimen

The fire effluent is passed through wash bottles, and the insoluble effluent is collected in a gas bag

The gases monitored include: carbon monoxide, carbon dioxide, sulphur dioxide, formaldehyde, ammonia, hydrogen cyanide, hydrogen chloride, hydrogen bromide, hydrogen fluoride, hydrogen sulphide, acrylonitrile and nitrogen oxides

Different methods are used for chemical analysis, e.g spectrophotometry, gas chromatography, infrared analysis and potentiometry.

Repeatability and reproducibility

Relevance of test data and special observations

The test temperature and ventilation conditions in this method do not align with any fire types listed in Table 1 However, by adjusting the test temperature or airflow rate, the physical fire model can be modified to accurately replicate fire types 2 or 3b, as detailed in Table 1.

The mass loss of the test specimen is not recorded during or after the test and, therefore, results cannot be expressed as toxic potency

Many physical fire models do not specify the combustion rate, allowing flame-retarded materials to burn at the same rate as non-retarded materials Consequently, for accurate fire hazard assessments, it is essential to gather additional data on combustion rates across various fire types.

A similar test, AFAP-3[11], has been developed by NATO, in which tests are carried out at

The analysis involves measuring various gases at temperatures of 350 °C and 800 °C with an air flow of 2 l × min -1 This includes the detection of carbon monoxide, carbon dioxide, hydrogen cyanide, hydrogen fluoride, hydrogen chloride, hydrogen bromide, nitrogen oxides, and sulfur dioxide Additionally, it requires the assessment of acrylonitrile, ammonia, phenol, benzene, styrene, and toluene under both temperature conditions, along with the measurement of hydrogen sulfide, formic acid, carbon disulfide, and acetaldehyde.

Reference documents

Norme Franỗaise (NF)

Summary

The NF C20-454 and NF X70-100 standards outline tests for determining the toxicity index of gases released during the combustion of test specimens in a tube furnace Specifically, NF C20-454 focuses on materials utilized in electrotechnical applications.

NF X70-100 was developed for testing products and materials used in the railway industry.

Purpose and principle

This tests measure and quantify the different gases evolved during the combustion or pyrolysis of test specimens

The gases monitored include: carbon monoxide, carbon dioxide, hydrogen chloride, hydrogen bromide, hydrogen fluoride, hydrogen cyanide, oxides of nitrogen (NO and NO 2 ), sulphur dioxide, formaldehyde and acrolein.

Test specimen

The test specimen, with a typical mass of 1,0 g, consists of a piece of material or a test specimen cut from an end-product.

Test method

The test specimen is placed in a porcelain boat inside a quartz combustion tube and introduced into an annular furnace set at 800 °C or, in the case of NF X70-100, 400 °C or

600 °C An air flow of 120 l × h –1 is passed through the tube, over the test specimen

A variety of analytical methods can be used, including chromatography, potentiometry, classical wet chemistry, IR and FTIR.

Repeatability and reproducibility

Data from interlaboratory testing are reported in NF X70-100-1 [14].

Relevance of test data and special observations

The test temperature and ventilation conditions in this method indicate that the physical fire model does not align with any of the fire types listed in Table 1 However, by adjusting the test temperature or airflow rate, the physical fire model can be modified to accurately replicate fire types 2 or 3b, as detailed in Table 1.

The mass loss of the test specimen is not recorded during or after the test and, therefore, results cannot be expressed as toxic potency

Many physical fire models do not specify the combustion rate, allowing flame-retarded materials to burn at the same rate as non-retarded materials Consequently, for accurate fire hazard assessments, it is essential to gather additional data on combustion rates across various fire types.

Results from NF X70-100 tests were compared with gas yields from full-scale fire tests of train materials, revealing reasonable correlations regarding the toxicity of structural materials.

NF X70-100 is one of the toxicity test methods specified in CEN TS 45545-2 [17]

NF X70-100 is discussed in ISO 16312-2.

Reference documents

International Electrotechnical Commission (IEC)

Summary

IEC 60695-7-50 outlines the process for generating fire effluent and identifying its combustion products This testing method employs a moving test specimen within a tube furnace, varying temperatures and airflow rates to simulate specific decomposition conditions across different fire types, as detailed in Table 1.

This test method closely models fire types 1b, 2, and 3b, as detailed in Table 1, while also having the capability to simulate additional fire types if needed The measurement of fire effluent is conducted using test specimens sourced from end-products, or, when feasible, the end-product itself.

Purpose and principle

The test method outlined aligns with the DIN 53436-1 standard and utilizes tube furnaces and quartz furnace tubes specified by IEC 60754-2, ensuring reliable performance under testing conditions and widespread availability.

In this test method, small pieces of a material strip are introduced into a quartz furnace tube at a constant rate, where primary air is passed through to support combustion The resulting effluent is expelled into a mixing and measurement chamber, diluted with secondary air, and subsequently analyzed before being evacuated.

The quartz furnace tube's decomposition conditions are established through various combinations of temperature and primary air flow rate during separate runs, aiming to simulate the decomposition conditions across different fire types as outlined in Table 1.

Test specimen

The test specimen is evenly distributed throughout the combustion boat, ensuring a consistent flow of decomposition products as it moves through the quartz furnace tube It is essential to maintain a combustible loading of about 10 g, evenly spread over a length of 400 mm.

Maintaining a uniform distribution of the test specimen is crucial, as is knowing the combustible loading per unit length, to accurately determine the rate of decomposition.

Test method

Each material should be tested under one or more of the decomposition conditions set out in Table 4:

3b Fully developed fire (flaming), relatively low ventilation 825 2,7

The furnace temperature is elevated to the desired level with a primary air flow rate, ensuring the air is clean and dry (relative humidity below 1% at 25 °C) The test specimen is evenly distributed on the combustion boat, which is then placed into the quartz furnace tube, positioned 50 mm from the air inlet A secondary air flow is adjusted to achieve a total flow rate of 50 l/min through the mixing chamber Calibration of the sampling and measurement equipment is completed before initiating the experimental run, during which the test specimen is moved through the quartz furnace tube at a speed of 40 mm/min.

Sampling of effluent

Samples for analytical measurement are continuously extracted from the chamber at a flow rate of 2 l × min –1 ± 0.05 l × min –1, passing through a drying agent and smoke filtration system before being analyzed Results are recorded continuously, including optional smoke optical density In flame experiments, observations are made through the quartz furnace tube to monitor ignition and ensure the absence of flames during non-flaming tests Fire conditions are verified through gas and smoke measurements, with outputs from the monitors closely observed in the early stages of the run.

Dynamic steady state conditions are achieved when constant levels are reached To accurately characterize the decomposition behavior of the test specimen and the yields of toxic products, the decomposition conditions must remain stable for at least 10 minutes.

Repeatability and reproducibility

Relevance of test data and special observations

Results of this test method can be used to estimate toxic potency based on the fractional effective dose (FED) principle as described in IEC 60695-7-51 [21]

Many physical fire models do not specify the combustion rate, allowing flame-retarded materials to burn at the same rate as non-retarded materials Consequently, for accurate fire hazard assessments, it is essential to gather additional data on combustion rates across various fire types.

Reference documents

International Standards Organization (ISO)

Summary

ISO/TS 19700 [22] is a tube furnace test method based on the IEC test method IEC 60695-7-50 The ISO test was first developed in the UK as BS 7990 [23].

Purpose and principle

Samples of a material or product are combusted under steady-state conditions in four distinct environments that reflect specific stages of a fire, characterized by their temperature and equivalence ratio These environments include oxidative pyrolysis, well-ventilated flaming developing fires, small flaming vitiated fires, and post-flashover vitiated fires, as outlined in ISO/TS 19706.

Test specimen

The test specimen is evenly distributed throughout the combustion boat, ensuring a consistent flow of decomposition products as it moves through the quartz furnace tube It is essential to maintain a combustible loading of about 20 g, distributed over a length of 800 mm.

(25 g × m –1 ) Preferably the test specimen should be in the form of a rod of uniform cross- sectional area.

Test method

Each material is tested under one of the following conditions as listed in Table 5

(see Table 1) Furnace temperature Primary air flow Equivalence ratio φ

2, well-ventilated flaming 650 °C 10 dm 3 × min –1 or

15 dm 3 × min –1 < 0,75 3a, small vitiated fire in a closed or poorly ventilated compartment 650 °C variable 2,0

3b, post-flashover fire in an open compartment 825 °C variable 2,0

Repeatability and reproducibility

Repeatability data are given for PMMA in ISO/TS 19700 Reproducibility had not been quantified when the ISO/TS 19700 was published.

Relevance of test data and special observations

Toxic potency data is available for fire types 1b, 2, 3a, and 3b The annexes in ISO/TS 19700 outline the application of this data in compliance with ISO 13344 and ISO 13571.

This test method requires preliminary assessments to establish the appropriate sample loading and air flow, ensuring that the desired fuel-to-oxygen equivalence ratios are met during steady-state decomposition While it is considered the most technically advanced standardized toxic potency test available, its complexity may be seen as a limitation.

Many physical fire models do not specify the combustion rate, allowing flame-retarded materials to burn at the same rate as non-retarded materials Consequently, for accurate fire hazard assessments, it is essential to gather additional data on combustion rates across various fire types.

BS 7990 is discussed in ISO 16312-2.

Reference documents

International Maritime Organization (IMO)

Summary

The IMO FTP [24] code smoke generation test is conducted in accordance with ISO 5659-

2 [25] Both smoke density and toxicity are measured during this test.

Purpose and principle

This mandatory test method evaluates surface finish materials on ships to ensure compliance with fire safety requirements outlined in the International Convention for the Safety of Life at Sea (SOLAS) 1974, as amended Specified in the International Code for Application of Fire Test Procedures (FTP Code) adopted by the IMO in resolution MSC 61 (67) in 1996, this method emphasizes the importance of using FTIR or another traceable analysis method for the chemical analysis of fire effluent.

Test specimen

The dimensions of the test specimen are 75 mm × 75 mm, as specified in ISO 5659-2 [25].

Test method

This test method follows ISO 5659-2 standards and is conducted for a minimum duration of 10 minutes If the minimum light transmittance value is not achieved, the test may be extended for an additional 10 minutes.

Three test specimens were evaluated under different conditions: a) with a pilot flame at an irradiance of 25 kW × m², b) without a pilot flame at the same irradiance of 25 kW × m², and c) without a pilot flame at a higher irradiance of 50 kW × m².

The results are expressed as gas volume fractions Maximum permitted values are given below (see Table 6):

Table 6 – Volume fraction limits for gas component

Gas component Limit of volume fraction × 10 6

Repeatability and reproducibility

Relevance of test data and special observations

The equivalence ratio varies throughout the test, and chemical analysis methods can be prone to errors and interferences Fire gases can accumulate in the upper section of the cabinet due to the absence of fan stirring, leading to potential deposition on soot and chamber walls Additionally, there is a lack of reported comparisons between toxic gas generation and data from real-scale fire tests.

Whilst relatively easy to perform, this method is of questionable value for generating effluent toxicity data for use in fire hazard analysis

A toxicity test using the same chamber is specified in CEN/TS 45545-2 [17]

Tests using this smoke chamber are discussed in ISO 16312-2.

Reference documents

Toxicity test for rolling stock cables

Summary

The test outlined in section 9.2 of EN 50305 [44] assesses the toxicity of combustion products generated from the complete burning of a small sample of material in excess air under defined conditions This material is sourced from the insulation, sheath, or other non-metallic components of a rolling stock cable.

The analysis is limited to materials classified as 'halogen-free' Quantitative assessments of sulfur dioxide and nitrogen oxides are conducted only after preliminary qualitative tests, specifically sodium fusion, confirm the presence of sulfur and nitrogen in the material.

NOTE ‘Halogen-free’ is as defined in Clause 3 of EN 50306-1 [45].

Purpose and principle

Analytical data of certain small molecular gaseous species arising from the combustion at

800 °C of the material under test are mathematically computed, using for each species a

‘critical concentration for a 30 min exposure’, to derive a combined toxicity index.

Test specimen

The test specimen is approximately 1 g and is a piece of the insulation or sheath or other non- metallic component taken from a rolling stock cable.

Test method

The apparatus is a tube furnace as described in EN 50267-1 [46]

The combustion tube operates at a temperature of 800 °C, where a test specimen is placed inside and air is circulated to facilitate combustion The resulting effluent is analyzed for carbon monoxide, carbon dioxide, and hydrogen cyanide Additionally, if the test sample contains sulfur, sulfur dioxide is measured, and if nitrogen is present, nitrogen oxides are also analyzed.

Air supply can be either pushed or pulled, with gas bags utilized to collect gases at the circuit's end when air is pulled Continuous analysis of carbon monoxide, carbon dioxide, hydrogen cyanide, and sulfur dioxide is achievable when air is pushed, while discontinuous analysis is possible for these gases and nitrogen oxides For detailed methods of analysis, refer to Annex E of EN 50305.

The results are expressed as a toxicity index, ITC, based on a weighted calculation as follows:

100g ⋅ m −3 m ∑(M z /CC z ) where m is the mass of the test specimen;

M z is the mass of gas z produced by the combustion of the test specimen, and

CC z is the critical concentration for a 30 min exposure of gas z (see Table 7)

Table 7 – CC z values taken from EN 50305

Repeatability and reproducibility

Relevance of test data and special observations

The test temperature and ventilation conditions in this method indicate that the physical fire model does not align with any fire types listed in Table 1 However, by adjusting the test temperature, the physical fire model can be modified to accurately replicate fire type 2.

The weighting values used in the calculation of the overall toxicity index are outdated

The mass loss of the test specimen is not recorded during or after the test and, therefore, results cannot be expressed as toxic potency

Many physical fire models do not specify the combustion rate, allowing flame-retarded materials to burn at the same rate as non-retarded materials Consequently, for accurate fire hazard assessments, it is essential to gather additional data on combustion rates across various fire types.

Reference document

7 Summary of published test methods relating to animal exposure

This summary does not replace published standards which are the only valid reference documents.

Deutsches Institut für Normung (DIN)

Summary

The DIN 53436 series of standards outlines a test method for thermally decomposing solid and liquid materials in a controlled air stream, allowing for the evaluation of the acute inhalation toxicity of the resulting thermal decomposition products.

Purpose and principle

This test method evaluates the thermal decomposition of materials in an air stream, focusing on the generation of toxic products It specifically assesses the inhalation toxicity of both decomposition and combustion byproducts.

Test specimen

Strip-like test specimens measuring 400 mm × 15 mm × 2 mm are used

For materials with a density less than 400 kg/m³, the thickness of the test specimen is adjusted to ensure that its mass per unit length (g/cm) matches that of a material with a higher density.

Test method

The apparatus is designed to continuously decompose a strip-like test specimen within a 1,300 mm long quartz tube, featuring an outer diameter of 40 mm and a wall thickness of 2 mm This tube is surrounded by a 100 mm long temperature-controlled annular furnace that moves at a rate of 10 mm per minute along the tube's axis As the furnace traverses the tube, it passes over the test specimen, which is placed in a quartz glass cuvette at the bottom Additionally, a variable stream of air is directed over the test specimen in the opposite direction of the furnace's movement.

The opposing movement of the furnace and airflow ensures that the hot decomposition gases do not preheat the undecomposed sections of the test specimen The test temperature ranges from 200 °C to 900 °C and is monitored using a reference body.

A 200 mm long steel rod, equipped with a welded thermocouple, is positioned in the test specimen holder to monitor temperature Three tests are conducted with a reference body at a consistent furnace temperature During the test, the effluent at the end of the quartz tube is cooled with fresh air, diluted, and directed into the inhalation chamber, exposing either the nose or the entire body of the rat Additionally, gas analysis can be performed throughout the testing process.

Repeatability and reproducibility

An evaluation of this method involving three laboratories has been performed [29], [30].

Relevance of test data and special observations

The DIN 53436-1 tubular furnace decomposition model has been utilized by various researchers to determine LC 50 (lethal concentration 50) data This physical fire model allows for the decomposition of materials in strip form under fire types 1b, 3a, and 3b conditions A consistent mass or volume of the tested material is decomposed under these specific conditions, enabling the easy acquisition of concentration response relationships by varying the concentration through the dilution of fire effluents with air.

This method effectively gathers toxicological data and gas yields from the combustion or pyrolysis of homogeneous materials It determines the lethal toxic potency data based on a 30-minute exposure under specific testing conditions Consequently, the toxicological findings can be correlated with the mass, volume, or surface area of the test specimen used.

Analytical calculations of LC 50 data can be performed using the concentration values of major fire gas components, significantly minimizing the need for animal testing.

Many physical fire models do not specify the combustion rate, allowing flame-retarded materials to burn at the same rate as non-retarded materials Consequently, for accurate fire hazard assessments, it is essential to gather additional data on combustion rates across various fire types.

No comparisons of toxic potency and gas yield data with real-scale fire test data have been published

This test method is discussed in ISO 16312-2.

Reference documents

National Bureau of Standards (NBS)

Summary

The "NBS Cup" furnace test is used for the assessment of the acute toxicity of inhaled combustion products.

Purpose and principle

This test method determines toxic potency by generating both flaming and non-flaming decomposition effluents in a static closed system It utilizes an electrically heated 1-liter cup-type crucible furnace connected to a 200-liter exposure chamber, which features six exposure ports for rats and provisions for effluent sampling and analysis.

The reported result is the LC 50 for a 30 min exposure plus a 14 day post exposure period, expressed as the mass of test specimen exposed per unit chamber volume.

Test specimen

The test specimen with a typical mass of up to 8 g can be a piece of material, or a test specimen cut from an end-product.

Test method

A 1-liter stainless steel electrically heated cup furnace is pre-set to a specific temperature, where a test specimen weighing between 1 g and 8 g is introduced The resulting effluent then fills the chamber through convection.

The article outlines two combustion modes: flaming and non-flaming In the non-flaming mode, the furnace temperature is maintained at 25 °C below the ignition temperature of the test specimen, while in the flaming mode, it is set at 25 °C above the ignition temperature The ignition temperature of the test specimen is established in the cup furnace before conducting the test.

The test is performed in a 200-liter clear plastic chamber that houses a cup furnace, with its open top level with the chamber floor, along with animal exposure ports and facilities for analytical sampling.

Rats are subjected to a 30-minute nose-only exposure to the atmosphere of a test chamber, starting with the introduction of the test specimen into the combustion chamber Those that survive this exposure are monitored for an additional 14 days, during which any deaths are attributed to exposure to combustion products and included in the determination of the LC 50 value.

Oxygen, carbon monoxide, and carbon dioxide levels are continuously monitored, with results reported as LC 50 for both flaming and non-flaming conditions This assessment involves a 30-minute chamber exposure followed by a 14-day observation period, with results expressed in milligrams of sample per liter of chamber volume The LCt 50 is determined by multiplying the LC 50 by the 30-minute exposure duration.

Other information recorded includes chamber conditions, maximum temperature and the concentrations of oxygen, carbon monoxide and carbon dioxide.

Repeatability and reproducibility

NBS reports indicate relatively good repeatability with this method.

Relevance of test data and special observations

The NBS test has now been largely superseded by the NIST (National Institute of Standards and Technology) test (see 7.3)

The NBS test faces criticism for its reliance on a cup furnace, which is optimized for homogeneous materials and struggles with composite or laminated specimens Additionally, the closed cup design can cause rapid temperature increases and oxygen depletion when testing large, highly combustible samples, potentially skewing the animals' responses to combustion products and compromising the validity of the results.

Characterizing the fire conditions for test specimens during decomposition can be challenging In a cup furnace, air enters only from the top, which means that larger, more combustible specimens may receive less oxygen compared to smaller or less flammable ones, potentially affecting their burn rate.

Carbon monoxide yields can fluctuate, and there is limited data comparing the toxic potency measured by this test method to that observed in full-scale conditions, leaving the practical implications of this limitation unclear.

The results are reported as mass concentration based on the amount of test specimen loaded, rather than the amount converted to volatile effluents Consequently, if the test specimen is not fully consumed, the reported results may overestimate the actual mass concentration in the fire effluent, leading to an underestimation of its toxic potency Although weighing the test specimen residue post-test and making appropriate corrections can address this issue, this step is not included in the published procedure.

This test method is discussed in ISO 16312-2.

Reference documents

National Institute of Standards and Technology (NIST)

Summary

The NIST radiant furnace method is employed for assessing toxic potency by generating both flaming and non-flaming decomposition effluents within a static closed system This method is referenced in NFPA 269 and ASTM E 1678 standards.

The lethal toxic potency is initially assessed using combustion atmosphere analytical data through FED calculations, aiming to reduce the necessity for animal testing in confirming biological responses.

The LCt 50 value from the N-gas model indicates the lethal concentration-time product for a 30-minute exposure followed by a 14-day post-exposure period This value is calculated by multiplying the mass loss of the test specimen by the exposure time per unit volume of the test chamber.

Purpose and principle

The combustion device consists of a horizontally mounted cylindrical quartz combustion cell,

130 mm inside diameter and approximately 320 mm in length It is connected to an animal exposure chamber through a stainless steel chimney, which is approximately

The combustion cell measures 30 mm × 300 mm × 300 mm and is equipped with four tungsten-quartz radiant heat lamps that focus on the test specimen A platform designed for test specimens measuring 76 mm × 127 mm and up to 51 mm thick is linked to a load cell beneath the combustion chamber, allowing for continuous mass monitoring of the specimen A high-energy spark serves as the ignition source.

Test specimen

The test specimen, typically weighing up to 8 g, can either be a material piece or a sample cut from a finished product The platform is designed to hold test specimens that measure 76 mm by 127 mm and can be up to 51 mm thick.

Test method

The NBS test utilizes a horizontally oriented combustion cell, replacing the traditional vertically oriented cup furnace This new design accommodates various test specimen geometries and features a load cell for continuous mass loss measurement A stainless steel chimney and shutter connect the combustion cell to the exposure chamber, allowing radiant heat from two externally mounted lamps to reach the specimen through quartz walls After 15 minutes of irradiation, the chimney shutter is closed, and the heat lamps are turned off.

In the initial phase of the test, no animals are involved; instead, a test specimen weighing approximately 5 g is subjected to radiant heat The effluent composition in the test chamber is continuously analyzed for carbon monoxide, carbon dioxide, oxygen, and other toxic gases predicted from the specimen's composition, such as organics and hydrogen cyanide The monitoring period for potential animal exposure lasts 30 minutes, with the final 15 minutes occurring with the lamps off and the chimney shutter closed After this period, the N-gas model and analytical data are utilized to determine the lethal Fractional Effective Dose (FED) of the effluent that animals would have experienced The specimen size is then adjusted to achieve a target FED of around 1.1, and the test is repeated for verification.

After establishing the correlation between test specimen size and FED, the procedure is repeated twice using the specified animals and exposure conditions for the NBS test In the initial test, the specimen size is modified to achieve an expected FED of 1.4 If the N-gas model accurately predicts toxic potency, one or two animals will die after the 14-day post-exposure period from the first test, while all six will perish in the second test Conversely, if the N-gas model fails to predict mortality, it indicates the presence of agents not accounted for in the model, necessitating the determination of the actual LCt 50 using standard toxicological techniques with the apparatus and animals.

Time-integrated chamber concentrations of carbon oxides are measured using infrared spectroscopy, while hydrogen halides and hydrogen cyanide are analyzed when necessary The minimum oxygen concentration in the chamber is assessed with a paramagnetic analyzer, and the mass loss of the test specimen is evaluated using a load cell.

The heat flux level of the test specimen exposure, the time to ignition of the test specimen and the extinction time for the flame are reported.

Repeatability and reproducibility

The NIST reports relatively good repeatability with this method, but no inter-laboratory evaluation of this method has been performed.

Relevance of test data and special observations

The NIST test provides LCt 50 values that serve as direct input for fire hazard calculations, addressing the limitations of the NBS test, particularly in terms of specimen accommodation and localized oxygen depletion Conducted under well-ventilated conditions, this test allows for the simulation of fire type 1b, provided the test specimen does not auto-ignite.

The test outlined in Table 1, specifically for radiant flux levels of 2, 3a, and 3b, is essential for acquiring quantitative data on the toxic potency of materials and end products, which can be utilized in fire hazard models.

Based on NIST research, it is claimed that post-flashover toxic potencies measured with this test agree with those from full-scale fires within approximately a factor of two [36]

The NIST test method acknowledges that chemical analysis may not reliably identify all toxic components in fire effluent Consequently, there have been initiatives to reduce the reliance on animal testing for assessing toxic potency, although complete elimination of animal use has not yet been achieved.

This test is discussed in ISO 16312-2.

Reference documents

University of Pittsburgh (Upitt)

Summary

The UPitt box furnace (described in reference [38]) can be used for measuring the toxic potency of products resulting from the decomposition conditions of developing fires.

Purpose and principle

This test method determines concentration response and toxic potency using a dynamic flow-through system It involves ramped heating of test specimens in a muffle furnace, which is linked to four exposure chambers for mice, equipped with sampling ports for effluent analysis.

This test method used to be required in the United States by the state of New York for certain construction, electrical and interior finishing materials and products.

Test specimen

Test specimens may consist of material pieces or samples taken from finished products The concentration of effluent is adjusted by altering the mass introduced into the furnace, usually ranging from 1 g to 10 g.

Test method

The test specimen is positioned on a load cell and subjected to decomposition in a furnace, where the temperature rises at a rate of 20 °C per minute starting from room temperature An air stream is drawn through the furnace at a flow rate of 11 liters per minute Once the specimen has lost 1% of its mass, the resulting effluent is mixed with additional air and directed into the animal exposure chamber.

The fire effluent is passed into a 4 dm 3 glass animal exposure chamber Analytical samples are taken from the exposure chamber

Mice are subjected to a 30-minute nose-only exposure to diluted effluent, starting the exposure period when weight loss in the test specimens is first observed Any animals that die during the test or within 10 minutes after exposure are included in the assessment of dose response and toxic potency.

Continuous analysis of oxygen concentration using paramagnetic methods, along with infrared measurement of carbon monoxide levels, enables the ongoing monitoring of various toxic combustion gases, including hydrogen halides and hydrogen cyanide, as necessary.

Repeatability and reproducibility

Multiple submittals of similar materials and products indicate that the repeatability of this test is very good.

Relevance of test data and special observations

The test method initiates in a non-flaming oxidative mode, eventually transitioning to a flaming state During this transition, the CO₂/CO ratios are typically low, often below 20:1 and frequently under 10:1, while temperatures remain below 600 °C These conditions do not align with the fire types outlined in Table 1, resulting in a lack of usable input data for fire hazard models.

Many physical fire models do not specify the combustion rate, allowing flame-retarded materials to burn at the same rate as non-retarded materials Consequently, for accurate fire hazard assessments, it is essential to gather additional data on combustion rates across various fire types.

LC 50 values have been reported and filed with New York State for over 15 000 products [39]

A significant finding is that 96% of the LC50 values are concentrated within a narrow range of less than one order of magnitude Specifically, 63.3% of these values lie between 5 g and 12.5 g, while an additional 32.7% fall within the range of 12.5 g to 28.1 g.

This test is discussed in ISO 16312-2.

Reference documents

Japanese fire toxicity test for building components

Summary

Under the revised Japanese Building Standards Law of 2000, fire safety evaluation and certification are conducted by organizations recognized by the Ministry of Land, Infrastructure, Transport and Tourism (MLIT) These organizations establish the methods and criteria for evaluation and certification, often employing a toxicity fire test that utilizes a combustion system similar to BS 476-6 In this test, the combustion effluent from the specimen is directed into a mixing chamber and subsequently into an animal exposure chamber, where the time taken for all eight mice to become incapacitated is recorded and compared to a specified time.

NOTE For this test, incapacitation is defined as the cessation of movement of both the mouse and the cage for a minimum of 30 s.

Purpose and principle

This article presents a comparative toxicity testing method for identifying semi-combustible and flame retardant materials in the construction industry, utilizing mice in gas exposure conditions The testing apparatus includes a furnace, a pre-mixing chamber, and an animal exposure chamber equipped with eight rotary cages.

Test specimen

The test specimen can be a piece of the material or a test specimen cut from an end-product measuring 22 cm × 22 cm × 1,5 cm maximum thickness The area exposed for testing is

Test method

The animal exposure chamber is maintained at a temperature of 30 °C, housing eight cages filled with mice Initially, a supplementary heat source heats the test specimen for 3 minutes, followed by the main heat source for an additional 3 minutes Combustion gas is introduced into the chamber at a rate of 10.0 liters per minute Monitoring continues for 15 minutes after the heating test begins, during which the time taken for each mouse to become incapacitated is recorded.

Test specimens are judged to have passed the test if the mean time to incapacitation exceeds a specified time.

Repeatability and reproducibility

In a study involving four laboratories and six materials, the inter-laboratory standard deviation for the time to incapacitation of mice was found to be below 15% Additionally, duplicate tests conducted within each laboratory demonstrated an agreement of within 5%.

Relevance of test data and special observations

The test method is rarely utilized today, as many recognized organizations agree that fire toxicity tests are unnecessary for materials with combustible content below established limits Additionally, materials with low combustibility or those that are fire-retarded are also exempt from these tests, as they are deemed to release minimal toxic effluents due to their low heat release characteristics.

The mass loss of the test specimen is not recorded during or after the test and, therefore, results cannot be expressed as toxic potency

The test method is useful for screening the incapacitation potency of fire effluent from various products, but the test conditions only simulate fires of type 3a (see Table 1)

This method is discussed in ISO 16312-2.

Reference documents

Japanese Ministry of Construction (JMC) [41]

Overview of toxicity test methods

See Table A.1 for an overview of toxicity test methods

Table A.1 – Overview of toxicity test methods

Type of test method Clause Test method

Could be adapted to provide toxic potency data

Relevant to fire types in Table 1

6.1 DS 02-713 No No No No No No No No

6.2 ABD 0031 No No No No No No No No

6.3 CEI 20-37/7 No Yes No No No No No No

NF X70-100 No Yes No No No a No No

6.5 IEC 60695-7-50 Yes N/A a Yes a Yes a Yes

6.6 ISO/TS 19700 Yes N/A a Yes a Yes Yes Yes

6.7 IMO FTP Code No Yes No Yes No No Yes No

6.8 EN 50305 clause 9.2 No Yes No No No a No No

7.1 DIN 53436 Yes N/A No Yes No No Yes Yes

7.2 NBS Cup furnace Yes N/A No Yes No Yes No No

7.3 NIST Radiant furnace Yes N/A No b No Yes Yes Yes

7.4 UPitt Box furnace Yes c N/A No No No No No No

7.5 Japanese test Yes N/A No No No No Yes No a It is possible to simulate this fire type, but not under the standard conditions of the test method b This fire type will be simulated provided that the test specimen does not auto-ignite c Toxic potency data can be calculated but the physical fire model does not correspond to any of the fire types of Table 1

Type of test method Clause Test method Comments

6.1 DS 02-713 This test method is now widely criticized The data from this test should not be used as input to toxic hazard assessments, fire hazard assessments or fire safety engineering calculations

6.2 ABD 0031 Fire and ventilation conditions do not allow a comparison between this physical fire model and any of the fire types described in Table 1

6.3 CEI 20-37/7 The test temperature and ventilation conditions in these methods are such that the physical fire model does not correspond to any of the fire types described in Table 1 However, with modifications to either the test temperature or air flow rate, the physical fire model could be made to replicate fire types 2 or 3b

Results of this test method can be used to estimate toxic potency based on the fractional effective dose (FED) principle as described in

The method is technically complex

Toxic potency data can be acquired under fire types 1b, 2, 3a, and 3b, as outlined in the annexes of ISO/TS 19700, which detail its application in line with ISO 13344 and ISO 13571 Although the IMO FTP Code method is straightforward to execute, its effectiveness in producing reliable effluent toxicity data for fire hazard analysis is questionable.

6.8 EN 50305 clause 9.2 With modification to the test temperature the physical fire model could replicate fire type 2

7.1 DIN 53436 The method is useful for obtaining toxicological data and gas yields from the combustion or pyrolysis of homogeneous materials

7.2 NBS Cup furnace The NBS test has now been largely superseded by the NIST test (see 7.3) 7.3 NIST Radiant furnace This is a useful test for obtaining quantitative toxic potency data for materials and end products for input to fire hazard models

7.4 UPitt Box furnace This test does not produce usable input data for fire hazard models

7.5 JMC The test method is useful for screening the incapacitation potency of fire effluent from various products, but the test conditions only simulate fires of type 3a a It is possible to simulate this fire type, but not under the standard conditions of the test method b This fire type will be simulated provided that the test specimen does not auto-ignite c Toxic potency data can be calculated but the physical fire model does not correspond to any of the fire types of Table 1

[1] Le Tallec, Y and Guillaume E., “Fire Gases and their chemical measurement” in

‘Hazards of Combustion Products’, Interscience Communications Ltd., London (2008)

[2] Ministry of Defence – Defence Standard 02-713 (NES 713) Issue 1, Determination of the toxicity index of the products of combustion from small specimens of materials

[3] Guillaume, E and Chivas, C., “Fire models used in toxicity testing” in ‘Hazards of Combustion Products’, Interscience Communications Ltd., London (2008)

[4] ABD 00031, Airbus Directives (ABD) and procedures – Fire – Smoke – Toxicity

IEC/TR 60695-6-30 provides guidance and test methods for assessing the obscuration hazards to vision caused by smoke opacity from electrotechnical products during fires This standard includes a small-scale static method for determining smoke opacity, detailing the necessary apparatus for accurate measurement.

[6] ASTM E-662, Standard Test Method for Specific Optical Density of Smoke Generated by Solid Materials

[7] AITM 2.0007, Airbus Industry Test Methods – Determinations of the specific optical smoke density of aircraft interior materials (JAR/FAR Part 25, Appendix F-Part V)

[8] AITM 2.0008, Airbus Industry Test Methods – Determinations of the specific optical smoke density of electrical wire/cable insulation

[9] AITM 3.0005, Airbus Industry Test Methods – Determination of specific gas components of smoke generated by aircraft interior materials

[10] CEI 20-37/7, Tests on gases evolved during combustion of electric cables and their compounds – Part 7: Determination of toxicity index of gases evolved during combustion of electric cables

[11] NATO AFAP-3, NATO Reaction to fire tests for materials toxicity of fire effluents – Ed 2,

[12] Hull, T R and Paul, K T., Bench-scale assessment of combustion toxicity – A critical analysis of current protocols, Fire Safety Journal, 42(5), 2007 pp 340 - 365

The NF C20-454 standard outlines essential environmental testing procedures, focusing on fire behavior and the analysis of gases released during the pyrolysis or combustion of materials used in electrotechnics It includes methods for assessing exposure to abnormal heat or fire, specifically utilizing the tube furnace method for testing.

[14] NF X70-100-1: 2006, Fire tests - Analysis of gaseous effluents - Part 1 : methods for analysing gases stemming from thermal degradation

[15] NF X70-100-2: 2006, Fire tests - Analysis of gaseous effluents - Part 2 : tubular furnace thermal degradation method

[16] Fire Standardisation Research in Railways (FIRESTARR), Final Report, European Standards, Measurement and Testing Programme, Contract SMT4-CT97-2164, Commission of the European Communities, Brussels, Belgium, 2001

[17] CEN TS 45545-2, Railway applications – Fire protection on railway vehicles – Part 2: Requirements for fire behaviour of materials and components

[18] IEC/TS 60695-7-50, Fire hazard testing – Part 7-50: Toxicity of fire effluent – Estimation of toxic potency – Apparatus and test method

[19] DIN 53436-1, Producing thermal decomposition products from materials in an air stream and their toxicological testing; decomposition apparatus and determination of test temperature (1981)

IEC 60754-2 outlines the testing methods for assessing the gases released during the combustion of electric cables, specifically focusing on determining the acidity of these gases This is achieved by measuring the pH and conductivity of the materials derived from the cables The standard was established in 1991 to ensure safety and compliance in electrical applications.

[21] IEC/TS 60695-7-51, Fire hazard testing – Part 7-51: Toxicity of fire effluent – Estimation of toxic potency – Calculation and interpretation of test results (2002)

[22] ISO/TS 19700, Controlled equivalence ratio method for the determination of hazardous components of fire effluents

[23] BS 7990, Tube furnace method for the determination of toxic product yields in fire effluents

[24] IMO FTP Code, International Code for Application of Fire Test Procedures (FTP Code) adopted by IMO as resolution MSC 61 (67) in 1996

[25] ISO 5659-2, Plastics – Smoke generation – Part 2: Determination of optical density by a single-chamber test (1994)

[26] ISO/TR 9122-5, Toxicity testing of fire effluents – Part 5: Prediction of toxic effects of fire effluents (1993)

[27] DIN 53436-2, Erzeugung thermischer Zersetzungsprodukte von Werkstoffen unter Luftzufuhr und ihre toxikologische Prüfung; Verfahren zur thermischen Zersetzung

[28] DIN 53436-3: Erzeugung thermischer Zersetzungsprodukte von Werkstoffen unter Luftzufuhr und ihre toxikologische Prüfung; Verfahren zu inhalationstoxikologischen Untersuchung (1989)

[29] Klimisch, H J., Hollander, H W and Thyssen, Comparative measurements of the toxicity to laboratory animals of products of thermal decomposition generated by the method of DIN 53436, J., J Comb Tox 7, 1980, pp 209 – 230

The study by Klimisch, Hollander, and Thyssen (1980) focuses on generating constant concentrations of thermal decomposition products within inhalation chambers It compares a method based on DIN 53436, specifically measuring carbon monoxide and carbon dioxide levels The findings are detailed in the Journal of Combustion Toxicology, providing valuable insights into inhalation exposure assessments.

[31] Hartzell, G.E., Overview of combustion toxicology Toxicology, 115, p.7-23, published by Elsevier Science Ireland for the National Fire Protections Association (NFPA) (1996)

[32] Levin, B.C et al., Further Development of a Test Method for the Assessment of the

Acute Inhalation Toxicity of Combustion Products, NBSIR 82-2532 Washington: US

The study conducted by Levin, Paabo, and Birky evaluates the National Bureau of Standards test method for measuring the acute inhalation toxicity of combustion products This interlaboratory assessment, documented in NBSIR 83-2678, was published by the US National Bureau of Standards in Gaithersburg.

[34] NFPA 269, Standard Test Method for Developing Toxic Potency Data for Use in Fire Hazard Modelling, NFPA International, Quincy, MA, USA

[35] ASTM E 1678, Standard Test Method for Measuring Smoke Toxicity for Use in Fire

Hazard Analysis, ASTM International, West Conshohocken, PA, USA

[36] Babrauskas, V., Harris Jr., R H., Braun, E., Levin, B C., Paabo, M and Gann, R G.,

The Role of Bench-Scale Test Data in Assessing Real-Scale Fire Toxicity, NIST

Technical Note 1284, National Institute of Standards and Technology, Gaithersburg,

[37] Alexeeff, G V et Packham, S C., Evaluation of Smoke Toxicity Using Concentration-

Time Products J Fire Sci 2(5): pp 362-379 (1984)

[38] Alarie, Y C and Anderson, R C., Toxicologic and acute lethal hazard evaluation of thermal decomposition products of synthetic and natural polymers, Toxicology and

[39] New York State Uniform Fire Prevention et Building Code, Article 15, Part 1120,

Combustion toxicity testing and regulations are essential for the implementation of building materials and finishes The Fire Gas Toxicity Data File, published by the New York State Department of State's Office of Fire Prevention and Control in 1986, provides critical information on the toxic effects of fire gases This resource is vital for ensuring safety standards in construction and fire prevention.

[40] Kaplan, H.L., Grand, A.F., Hartzell, G.E., Combustion toxicology – Principles and test methods Technomic Publishing Co., Box 5535, Lancaster Pennsylvania 17604, USA

[41] Tsuchiya, Y., New Japanese standard test for combustion gas toxicity, Journal of Combustion Toxicity 4, pp 5-7 (1977)

[42] Saito, F., Toxicity test for fire resistive materials in Japan, Journal of Combustion Toxicology, 9, 1982, pp 194 - 205

[43] BS 476-6, Fire tests on building materials and structures – Part 6: Method of test for fire propagation for products (1989)

[44] EN 50305:2002, Railway applications - Railway rolling stock cables having special fire performance - Test methods (Clause 9.2, Toxicity Annex E, Analysis methods for toxicity)

[45] EN 50306-1:2002, Railway applications - Railway rolling stock cables having special fire performance – Thin wall – Part 1: General requirements

[46] EN 50267-1:1999, Common test methods for cables under fire conditions – Tests on gases evolved during combustion of materials from cables – Part 1: Apparatus

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