Control ed equi valenc e ratio method for the determination This document desc ibes a st eady-s at e tube furnac SSTF method for the g ene ation of fir ef luent for the identif ication
Trang 1Control ed equi valenc e ratio method
Méth de du ra p rt d’é uivalenc co trôlée p ur la déte mination
des substa ce s da ge euse s de s effluent du feu — Fo r tu ulaire à
Trang 2COPYRIGHT PROTECTED DOCUMENT
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Trang 3F reword v
Introduction vi
1 Sc ope 1
2 Nor mati ve r eferenc es 2
3 Terms and definitions 2
4 Principle 3
5 A pparatus 4
5.1 General a p r atus 4
5.2 T ubular furnac 4
5.3 Calbrated the mocouples 6
5.4 Q uartz furnac tube 6
5.5 Combustion b at 6
5.6 Combustion b at drive 7
5.6.1 Me hanism 7
5.6.2 Rate of spe imen intr od ction 7
5.7 Mix ing an measur ement chambe 8
5.8 A nalysis of gases 8
5.9 Dete mination of smoke aer osols 1
5.1 Ex haus sys em 1
6 A ir supples 10
6.1 Primary an se on ary air supples .1
6.2 Primary airflow calbration 1
6.3 S con ary airflow calbration 1
6.4 Overal confirmation 1
7 Establshment of fur nac e temperatur e and set ing of fur nac e temperatur e 11
7.1 General 1
7.2 Establshing furnac temperatur e pr ofie to dete mine furnac suitabi ty 1
7.3 S tting the temperatur e for an in ivid al tes ru con ition 1
8 Test specimen pr eparatio 13
8.1 Tes spe imen form 1
8.2 Combustible lo ding 1
8.3 Spe imen conditioning 1
9 S lection of test dec ompositio c onditions 13
9.1 S le tion of de omp sition con itions for fire hazar d analysis or fire safety eng ine ring 1 9.2 Stag e 1 ):ox idative pyrolysis fr om ex te naly a pled r adiation 14
9.3 Stag e 2:wel-ventilated flaming 14
9.4 Stag e 3 ): smal vitiated fires in closed or po r ly ventiated comp rtments 1
9.5 Stag e 3 ):pos -flasho e fir es in o en comp rtments 1
10 Proc ed re .16
1 1 Safety considerations 1
1 2 De omp sition of the tes spe imen 1
1 3 Stead y-s ate pe iod 1
1 4 Sampl ng an analysis of fire efluent 1
1 4.1 General 1
1 4.2 Samplng of fire efluent 1
1 4.3 Dete mination of the mas of the spe imen resid e 2
1 4.4 A mbient con itions 2
1 5 Valdity of tes ru 2
11 Calculations .21
Trang 41 2 Mas -char g e conc ntration an mas -los conc ntr ation 2
1 2.1 Mas -char g e conc ntration 2
1 2.2 Mas -los conc ntration 2
1 3 Yield 2
1 4 Or ganic fraction 24
12 Test rep rt 24 1 1 Content of tes r eport 24
1 2 Tes la or atory detais 2
1 3 Spe imen detais 2
1 4 Tes con itions an pr oc d res 2
13 Verification of test apparatus w ith PMMA 26 1 1 Pr oc dur e 2
1 2 Ve ification c ite ia 2
14 Tr uenes and unc ertainties w ith r espect to ste dy-state tube furnac e c onc entration and yields 26 14.1 Accuracy, truenes an u c rtainty 2
14.2 Accuracy an truenes of conc ntr ation an yield measur ement in the s eady-s ate tube furnac (S TF) 2
14.3 Ex tent of v ria i ty of conc ntr ation an yield measur ement fr om tes spe imens in the s eady-state tube furnac 2
14.4 Correlation of efluent yields fr om the s eady-s ate tube furnac with those o tained fr om lar g e-scale comp rtment fir e tests u de the same combustion con itions 2
15 Repe tabiity and reprod cibiity 28 A nne x A (informative)Guidanc e o the ch ic e of additional decomp sitio c onditio s 30 A nne x B (informative)Estimation of lethal tox ic potency for c omb stio pr oducts ac c or ding to ISO 13344 using tube-furnace data 32 A nne x C (informative) A ppl cation of data fr om the tu e-furnac e test to estimatio and as es ment of tox ic hazar d in fir es ac c ording to ISO 135 1 33 A nne x D (informative) Use of the tube-fur nac e metho for bioas ay purposes 34 A nne x E (informative) Me surement of o tical density fr om the ste d y-state tube fur nac e .35 A nne x F (informative) C mpar iso of data fr om the ste dy-state tube furnac e, the ISO 9705 room and othe compar tment fir e ex periments 37 A nne x G (informative) A sses ment of mas - os rate data 41
Biblog raph y 46
Trang 5ISO (he Int ernational Org nization for Stan ardization) is a worldwide fede ation of national s an ards
b dies (ISO membe b dies) The work of pr p ring Int ernational Standards is normaly car ied out
through ISO t ech ical committ ees Each membe b dy int er st ed in a subje t for w hich a t ech ical
committ ee has be n es a l shed has the right t o be r pr sent ed on that committ ee Int ernational
org nizations, g ove nmental an non-g ove nmental, in laison with ISO, also take part in the work
ISO cola orat es closely with the Int ernational Ele trot ech ical C mmis ion (IEC) on al matt ers of
ele trot ech ical s an ardization
The proc d r s used t o develo this document an those int en ed for it furthe maint enanc ar
desc ibed in the ISO/IEC Dir ctives, Part 1 In p rticular the dife ent a pro al c it eria ne ded for the
dife ent ty es of ISO document should be not ed This document was draft ed in ac ordanc with the
edit orial rules of the ISO/IEC Dir ctives, Part 2 ( e www.iso.org dir ctives)
A tt ention is drawn t o the p s ibi ity that some of the element of this document ma be the subje t of
p t ent right ISO shal not be held r sponsible for identifying any or al such p t ent right Detais of
any p t ent right identif ied d ring the develo ment of the document wi be in the Introd ction an / r
on the ISO ls of p t ent de larations r c ived ( e www.iso.org p t ent )
Any trade name used in this document is information given for the convenienc of use s an does not
cons itut e an en orsement
For an ex lanation on the meaning of ISO spe ific terms an ex r s ions r lat ed to conformity as es ment ,
as wel as information a out ISO’s adhe enc to the Wor ld Trade Org nization (WTO) principles in the
Te h ical Bar ie s to Trade (TBT) se the folowing URL: www.iso.org iso/ for word.html
The committ ee r sp nsible for this document is ISO/TC 9 , Fir s afet y, Subcommitt ee SC 3, Fir thr at
to peo le a d env iro ment
This se on edition canc ls an r plac s the f irs edition (ISO/TS 1 7 0:2 0 ), w hich has be n
t ech icaly r vised
The chang es in this document ar as folow s
— The int erla orat ory r prod cibi ity has be n as es ed with homog enous the mo las ic mat erials
— A ve ification proc d r of the t es a p ratus with PMMA has be n introd c d
— A new se tion on truenes an unc rtainties with r spe t t o st eady-s at e tube furnac conc ntration
an yields has be n ad ed
— A new se tion on r peata i ity an r prod cibi ty has be n ad ed
— New informative an ex es ha e be n ad ed ( e An ex es F an G)
— The l s of r fe enc s has be n updat ed
Trang 6Fir safety engine ring using pe formanc -based design r q ir s engine ring methods for spe ific
pe formanc aspe t of fir safety, but a plca le t o al ty es of s ructural sy st ems, prod ct an
proc s es This inclu es s an ard t es methods for o taining data on spe if ic fir -r lat ed phenomena
inclu ing the g ene ation of harmful fir ef luent These ha e be n designed t o pro ide the input data
ne es ary for engine ring calculation methods for phy sical, chemical an biolo ical pro e ties The
ex osur con itions an pe formanc ne d t o be adeq at ely q antif ied t o alow extra olation from
t es con itions t o dife ent f ir situations oc ur ing in the r al world
The t oxic hazard t o an oc upant of a buiding or transport enclosur d ring a f ir depends on ex osur
t o the time-v rying conc ntrations of t oxic prod ct (g ses an smoke particulat es) in each oc up nt’s
br athing zone, the efe t of each t oxicant an the int eractions betwe n them The conc ntrations of
t oxic g ses an particles depen primari y on the mas -los rat e of the fuel, the yields of each t oxicant
an the dynamics of air entrainment an ef luent dispe sal within the oc upied enclosur () Othe
fact ors, such as los es from dep sition on the walsof the enclosur , ma also ne d t o be conside ed
F or fir safety calculations, such as those desc ibed in ISO 1 7 2-1
[1]
the yields of t oxic prod ct from
the burning fuel ar ne es ary input Sinc combus ion con itions v ry d ring a fir an betwe n
dife ent f ir s, it is also ne es ary t o measur the t oxic prod ct yields u de a rang e of def ined
combus ion con itions In orde t o make a pe formanc -b sed as es ment of the t oxic hazard in a
fir , yield data of t oxic prod ct un e dife ent pe ified fir con itions comprise one cat eg ory of the
r q ir d input
F or any spe if ic mat erial, the ef luent yields in fir s depen up n the the mal de omp sition con itions
Themos important v ria les ar w hethe the de omp sition is non-flaming or flaming, an for flaming
de omp sition, the fuel/ xyg en ratio Based up n these v ria les, it is p s ible t o clas ify f ir s int o a
n mbe of ty es, asdetaied in ISO 1 7 6:2 1 , Ta le 1
This method has be n develo ed t o measur t oxic prod ct yields from mat erials over a rang e of defined
de omp sition con itions in f ir s A t this s ag e, the int erla orat ory r prod cibi ty has be n as es ed
with homog enous the mo las ic mat erials, an this document is the efor l mit ed in a plca i ty
t o such mat erials The de omp sition con itions ar def ined in t erms of fuel/ ir eq iv lenc ratio,
t empe atur an flaming beha iour
The method has be n shown t o r plcat e the prod ction yields of t oxic f ir ef luent in a n mbe of
s u ies for a rang e of p lyme s, desc ibed in 14.4 and Annex F
The use of this document pro ides data on the rang e of t oxic prod ct yields lkely t o oc ur in
dife ent ty es an s ag es of ful-scale fir s Mor compr hensive data on the r lationships betwe n
de omp sition con itions an prod ct yields can be o tained b using a wide rang e of a p ratus
set ings Guidanc on the choic of ad itional de omp sition con itions is given in An ex A The
es imation of lethal t oxic p t ency data ac ording t o ISO 1 34 is desc ibed in An ex B The use of data
t o as es t oxic hazard ac ording t o ISO 1 5 1 is desc ibed in An ex C Guidanc on the a plcation of
data for bio s a purposes is desc ibed in Annex D
The t es method has be n develo ed t o fulf il the r q ir ment of ISO 1 3 2-1 an ISO 1 7 6, for data
on the yields of t oxic prod ct in f ir efluent evolved u de dife ent f ir con itions as p rt of the
data r q ir d for input t o the t oxic -hazard-as es ment calculation methods desc ibed in ISO 1 5 1
The data ma also be used as input for the t oxic -p t ency calculation methods desc ibed in ISO 1 34
an ISO 1 5 1
Trang 7Control ed equi valenc e ratio method for the determination
This document desc ibes a st eady-s at e tube furnac ( SSTF) method for the g ene ation of fir ef luent
for the identif ication an measur ment of it cons ituent combus ion prod ct , in p rticular, the yields
of t oxicant u de a rang e of fir de omp sition con itions
It uses a mo ing t es spe imen an a tube furnac at dife ent t empe atur s an airflow rat es as
the fir model The int erla orat ory r prod cibi ity has be n as es ed with sele t ed homog enous
the mo las ic mat erials and this document is the efor lmit ed in a pl ca i ity t o such mat erials The
method is v ldat ed for t es ing homog eneous the mo las ic mat erials that prod c yields of a def ined
consist ency S e lmitations in Clause 1
This method has be n designed as a pe formanc -b sed engine ring method t o pro idedata for input t o
hazard as es ment and fir safety engine ring design calculations The method can be used t o model a
wide rang e of combus ion con itions b using dife ent combinations of t empe atur , non-flaming an
flaming de omp sition con itions an dife ent fuel/ xy g en ratios in the tube furnac These inclu e
the combus ion con itions for the folowing ty es of f ir s, as detaied in ISO 1 7 6:2 1 , Ta le 1:
— Stag e 1: Non-flaming:
— Stag e 1 )Oxidative p roly sis from ext ernaly a pled radiation;
— Stag e 2: Wel-ventiat ed flaming (r pr senting a flaming develo ing f ir );
— Stag e 3: Un er-venti at ed flaming:
— Stag e 3a) Smal local z d fir s in closed or p orly venti at ed compartment ;
— Stag e 3 )Pos -flasho e fir s
F or each flaming fir ty e, the minimum con itions of t es ar spe if ied in t erms of the eq iv lenc
ratio, ϕ, as folow s:
Stag es 3 ) an 3b) ϕ =2 ± 0,2
Guidanc on the choic of ad itional de omp sition con itions is given in Annex A
The data on t oxic prod ct conc ntrations an yields o tained using this document can be used as p rt
of the es imation of t oxic p t encies, in conju ction with t oxic p t ency calculation methods in ISO 1 34 ,
an as an input t o the t oxic hazard as es ment from fir s in conjunction with fir growth an ef luent
dispe sal model ing, an fractional efe tive dose(FED ) calculation methods in ISO 1 5 1
Ap lcation of data from the st eady-s at e tube furnac t o the es imation of lethal t oxic p t ency and t o
the as es ment of t oxic hazards in fir s is conside ed in Annex B an An ex C, r spe tively Guidanc
on a plcation of data from the st eady-s at e tube furnac t o the use of the st eady-s at e tube furnac
method for bio s a purp ses is given in An ex D
The t es method desc ibed in this document can beused solely t o measur an desc ibe the prod ction
of t oxic ef luent from homog eneous the mo las ic mat erials, in r sp nse t o heat or flame un e
controled la orat ory con itions It is not suita le t o be used, b it elf, for desc ibing or a praising
Trang 8the fir hazard of mat erials u de actual fir conditions, or as the sole sour e on w hich r gulations
pe taining t o t oxicity can be b sed
The yields of combus ion prod ct det ermined using thisdocument pe tain t o the time int erv l d ring
w hich st eady-s at e burning is o se ved To the ext ent that this int erv l is not a larg e fraction of the
t otal burning time ( i.e if les than 5 min), the st eady-s at e yield v lues ar a plca le with caution t o
fir safety analy ses
2 Normati ve referenc es
The folowing document ar r fe r d t o in the t ext in such a wa that some or al of their cont ent
cons itut es r q ir ment of this document F or dat ed r fe enc s, only the edition cit ed a ples F or
un at ed r fe enc s, the lat es edition of the r fe enc d document ( inclu ing any amendment ) a ples
ISO 2 1, Plas tic s — Sta dard atmos phe es fr c onditio in a d tes tin
ISO 1 8 8-1, Valdatio meth d fr fir g s a alys i s — Part 1: Limits o detec tion a d q a tific atio
ISO 1 8 8-2, Vali dati on meth d fr fire g s a al ysis — Par t 2: Intralab ratory v lidation o
q a tification meth d s
ISO 1 344, Es timatio o the leth l tox ic p tency o fir effluent
ISO 1 5 1, Life -thr atenin c omp nents o fir — Guidelnes fr the es timatio o time to c ompromi s ed
ten bi t y in fir s
ISO 1 7 1, Meth ds fr s ampln a d a alys i s o fir effluents
ISO 1 7 2, Guida c e fr s ampln a d a alys i s o toxic g ses a d v p urs in fir effluent us in Fo rie
Tra s form In rar d (FTIR) s pec trosc op
ISO 2 9 3, Guida c e f r c omp ri s on o tox ic g s data bet we n dife ent p ys ic al fir model s a d sc ales
ISO/IEC G ide 9 -3, Unc ertaint y o meas ur ment — Part 3 : Guide to the expr s s io o u c ertaint y in
meas ur ment (GUM:19 9 5)
3 Terms and definitions
F or the purposes of this document, the t erms an definitions given in ISO 1 344, ISO 1 5 1, ISO 1 943,
an the folowing a ply
ISO an IEC maintain t erminolo ical data ases for use in s an ardization at the folowing ad r s es:
— IECEle tro edia: a aia le at ht p:/ www.ele tro edia.org
— ISO Onlnebrow sing plat orm:a ai a le at ht p:/ www.iso.org o p
3.1
ac uracy
ext ent t o w hich the measur d v lue r pr sent thetrue v lue, inclu ing the v ria i ity an u c rtainties
of the measur d v lue
Not e 1 to entry: T e e tent t o which yields me sured in the tub furnace for a specimen are predictive of
the yields oc ur ing when specimens are decomposed u der the same combustion con ition in larg -s ale
compartment f ire tests des rib s ac uracy in this case
Not e 2 to entry: Def inition of the ac uracy of a me sured value of a prod ct concentration or yield from a tub
furnace test ru , se also Clause 14
Trang 9steady-state b rning co ditio s
combus ion of fuel at a cons ant rat e u de cons ant venti ation, pro iding cons ant combus ion
con itions
Note 1 t o entry: T e ste d -state tub furnace is designed t o combust t est specimens u der ste d -stat e
con itions, by introd cing fuel int o the furnace at a constant rat e u der a constant flow of air During a test
ru , ste d -state con itions can b conf irmed by contin ous me surement of the carb n dio ide an o y gen
concentrations T e c iteria of ste d -stat e combustion con itions using this method are def ined in 1 3
The yields of combus ion prod ct from fir s depen up n the de omp sition con itions
[2][3][4][5]
[6]
The spe ified t es con itions ha e be n chosen t o r plcat e o idative p roly sis u de non-flaming
con itions, wel -venti at ed flaming con itions at an eq iv lenc ratio of les than 0,7 , un er-ventiat ed
pr -flasho e flaming con itions and pos -flasho e u der-venti at ed flaming conditions, b th at
an eq iv lenc ratio of aroun 2 as defined in ISO 1 7 6 The t es is designed t o combus mat erials
un e a rang e of con itions, dife ent fuel/ ir eq iv lenc ratiosan t empe atur s This t es combus s
mat erials u de defined con itions with r spe t t o non-flaming an flaming combus ion, dife ent
fuel/ ir eq iv lenc ratios an t empe atur s ex e ienc d in r al f ir s as def ined in ISO 1 7 6 It is
es ential that pro e o se v tions ar made d ring t es ing t o ensur that the spe if ied con itions ar
being met
Spe imens ofa mat erial ar combust ed u de one or mor steady-s at e con itions whose t empe atur
an eq iv alenc ratio ar r pr sentative of a p rticular s ag e of a fir A t es spe imen ( in the form
of gran les or pelet , or as a contin ous mat erial) is uniformly dis ribut ed along an 8 0 mm q artz
combus ion b at This is introd c d at a cons ant rat e int o a q artz furnac tube w hich pas es through
a fixed tubular furnac A s r am of primary air is p s ed through the q artz furnac tube an o e the
t es spe imen at cons ant flow The t es spe imen is driven into the hot zone of the tubular furnac Un e
flaming con itions, ignition oc urs, then the flame s a i z s, burning the tes spe imen at a fixed rat e,
in the pr senc of a controled flow of primary air The fir efluent mo es through the q artz furnac
tube int o a mixing an measur ment chambe w he e it is diut ed with se on ary air, giving a t otal flow
of (5 ± 1) dm
3
⋅min
−
through the chambe , and is then exha ust ed t o the fume extraction sy st em
In o idative p roly sis con itions, the furnac t empe atur is set below the aut o-ignition t empe atur
The thr e flaming con itions ar ac omplshed b using furnac t empe atur s a o e the aut o-ignition
t empe atur F r flaming de omp sition con itions, dife ent, cons ant primary airflow s ar used at a
cons ant rat e of introd ction of the t es spe imen t o o tain dife ent fuel-t o-o yg en ratios, an henc
dife ent eq iv lenc ratios
The se on ary, diution air g ene ates a gr at er sample flow an co le efluent w hich pe mit a larg e
n mbe of g s an smoke samplng proc d r s t o be used without the ne d for ad itional r plcat e t es s
The r q ir ment in each t es ru is t o o tain s a le, st eady-s at e de omp sition con itions, for at leas
5 min, or long er if p s ible, d ring w hich the conc ntrations of efluent g ses an p rticles shal be
measur d The time taken for st eady-s at e con itions t o be es a l shed v ries, depen ing upon the
natur of the t es spe imen and the t es con itions
The conc ntrations of carb n dio ide an o y g en ar r corded contin ously t o identify the pe iod in
w hich st eady-s at e burning con itions oc ur an samples of the ef luent mixtur ar taken from the
chambe d ring the st eady-s at e pe iod for analy sis A sample of smoke shal be drawn through a f ilt er
Trang 105 A pparatus
5.1 General apparatus
The a paratus consis s of a tubular furnac an a q artz furnac tube w hich pas es through the furnac
an int o a mixing an measur ment chambe A drive me hanism pushes the combus ion bo t int o the
q artz furnac tube at a pr -set, controled rat e A cons ant, k own flow of primary air mo es through
the q artz furnac tube, o e the mo ing t es spe imen, t o the mixing an measur ment chambe A
controled se on ary sup ly g oes dir ctly int o the mixing an measur ment chambe Gaseous samples
ar taken from the mixing an measur ment chambe
The ar angement of the a pp ratus is shown in Figur 1 Unles othe wise s at ed, al tole anc s ar ± mm
NOTE A light/p ot o cel syst em can b used t o determine smoke density ac os the mixing an me surement
chamb r (se An e E)
5.2 T ubular fur nac e
The tubular furnac shal ha e a heating zone length of 5 0 mm t o 8 0 mm an an inside diamet er of
5 mm t o 6 mm The furnac shal be eq ip ed with an adjus a le ele tric heating sy st em ca a le of
r aching 1 00 °C an maintaining the furnac t empe atur t o within ± % of the set t empe atur with
an empty q artz furnac tube in plac u de s atic con itions
The heating element should pr fe a ly be rat ed at 1 3 0 °C The furnac is simiar t o that used in
IEC 6 7 4– 2
W ith the peak furnac t empe atur set at (6 0 ± 1 ) °C, the t empe atur shal not de r ase b mor
than 1 0 °C o e a length of at leas ± 2 mm from the point of peak t empe atur measur ment The
method used t o det erminethis t empe atur prof ile is given in 7.2
NOTE This wil also red ce the likeliho d of a hot spot in the furnace, t o which the p roly sis rate wil b
sensitive
Trang 11Dimensions in milimetr es
a) General ar ang ement of apparatus
b)Critical dimensions of as embly
Key
4 combustion b at drive mechanism 1 p mp w ith flow meter (optional, for gas bub ler )
5 mix ing an me sur ement chamb r 14 secon ary air inlet 45° to vertical
8 ports for sampling lines 17 combustion b at 8 0 mm long
9 smoke-particle filter
Figure 1 — Tube-furnace decompositio and samplng apparatus
Trang 125.3 Cal brated thermoc ouples
Calbrat ed s ainles -st eel sheathed the mocouples, (1,5 ± 0,1) mm in diamet er, shal be used for
measuring the t empe atur in the furnac tube, the t empe atur in the mixing and measur ment
chambe an for calbrating the furnac
5.4 Quartz furnace tube
The q artz furnac tube, as shown in Figur 2, is made of clear heat-r sis ant q artz, r sis ant t o the
efe t of fir ef luent The tube shal be long enough t o ac ommodat e the combus ion b at out ide the
furnac , t o p s through the furnac an protru e int o the mixing an measur ment chambe at the
far en of the furnac The tube shal the efor be at leas (furnac length + 8 5 mm) in length It has
an ext ernal, a pro imat ely conc ntric diamet er of (47,5 ± 1) mm an a wal thick es of (2 ± 0,5) mm
The out ide diamet er shal pe mit a smo th f it within the tube furnac (5.2) an alow ex ansion at
o e ating t empe atur s
The input en of the furnac tube shal have a closur with o enings in it t o alow the primary air inlet
an the combus ion b at drive t o p s through w hi e maintaining a leak-pro f seal
NOTE 1 A polytetrafluoro th lene (P F )glan se l has b en fou d to b suita le
The downs r am en of the furnac tube shal p s through a heat-r sis ing sealed glan an shal
protru e5 ± 5 mm int o the mixing an measur ment chambe (5.7)
NOTE 2 A glan made from glas wool or from glas rope inside a metal colar has b en fou d to b suita le
The en of the furnac tube should be a le t o ac ommodat e an airflow r s rict or r d cing the outlet
diamet er of the q artz furnac tube t o the mixing an measur ment chambe t o a ma imum ar a of
b rosilicate glas la orat ory b aker which
f its sn gly inside the furnace tub , with a 3 mm diamet er cir ular hole cut int o the b se.T e hole was cut with
the b aker u der water, using a low voltag e “Dremel” dril an grin ing bit
The dis anc betwe n the exit of the tubular furnac an the mixing an measur ment chambe shal
be (3 ± 5) mm
The q artz furnac tube shal be horizontal (within ± mm in the ve tical dir ction pe metr along the
furnac a is) t o ensur that molt en fuels can ot flow upor down the combus ion b at d ring a ru
5.5 Combustion boat
The combus ion b at, as shown in Figur 2, is made from q artz tubing of diamet er (41± 1) mm, with a
length of 8 0 mm an a wal thick es of (2 ± 0,5)mm Theb at should be cleaned aft er each t es
NOTE 1 A suita le combustion b at has b en made from q artz tubing with a nominal diameter of 41 mm
This was sliced in half along its a is t o provide a semicir ular c os -section,nominaly of 41 mm width,1 mm
depth an 8 0 mm length Flat semicir ular q artz plat es were fused ont o e ch en
NOTE 2 A b at diameter (41 mm)provides the ma imum test specimen capacity
A bo t length of 80 mm has be n fou d suita le for t es ing mos mat erials Whe e mat erials take a
long time t o r ach st eady-s at e burning, or w he e a st eady-s at e pe iod of long er that 5 min is r q ir d,
long er b at ma be used
NOTE 3 A convenient method of cle ning b th the b at an tub is t o remove o vious resid es mechanical y,
then he t in a furnace at 1 0 0°C, fol owed by washing in water t o remove an inorg nic resid es
Trang 135.6 Combustion boat dr i ve
5.6.1 Mechanism
The combus ion b at is conne t ed t o a not ched drive b r, w hich p s es through the glan seal (5.4)
at the ups r am en of the furnac tube, an conne t t o a drive me hanism The drive me hanism
adv nc s the b at at a ty ical rat e of (40 ± 1) mm·min
−
The drive me hanism shal alow dife ent
adv nc rat es t o be sele t ed
The ca acity of the drive me hanism shal be sufficient t o mo e the combus ion b at at leas 80 mm
This wi mo e the front of the b at from the near en of the furnac al the wa t o the far en of the
furnac , jus alowing the r ar en of the 8 0 mm b at t o ent er the furnac The me hanism shal ena le
the b at t o be ra idly r tract ed int o the ups r am, ext ernal part of the furnac tube at the en of the
t es run Thisma be achieved man aly aft er detaching the push rod from the drive me hanism
A drive adv nc rat e of 40 mm ⋅min
−
has be n fou d suita le for mos mat erials un e mos
de omp sition con itions F or some fas -burning or low-density mat erials, it has be n fou d ne es ary
t o use adv nc rat es of up t o 6 mm·min
−
F or t es s inv lving spe imens of uniform lnear density,
such as rods of mat erial, the drive adv nc rat e should be adjust ed t o give a fuel fe d rat e of 1 g·min
−
5.6.2 Rate of specimen introductio
The rat e of introd ction of the combus ion b at ( in mm·min
−
) shal be det ermined b adv ncing the
b at o e a dis anc of ( 80 ± 1) mm an measuring the time taken This is (1 2 0 ±1 ) s at an adv nc
rat e of (40 ± 1) mm·min
−
The mos imp rtant c it erion for this p ramet er is r peata i ity, w hich
should be within ± % The actual adv nc rat e ma be up t o 1 % highe or lowe than the spe ified
rat e The actual adv nc rat e shal be measur d t o 1 % ac uracy an the spe imen mas lo ding is
adjust ed t o pro ide a mas fe d rat e eq iv lent t o that spe if ied ( e 9.2 an 9.3)
Dimensions in milimetr es
a) Quartz furnace tube
b) C mbustion boat
Figure 2 — Dimensio s of a suitable quartz furnace tube and combustio boat
Trang 145.7 Mix ing and measur ement chamber
The mixing an measur ment chambe shal be an a pro imat ely cubic bo with a side length of
(3 ± 2) cm ( e Figur 3), although the ex ct dimensions ar not c itical The front of the chambe has
a do r, pro iding a seal w hen sh t, but ena l ng cleaning of the chambe w hen o en
NOTE 1 The wals of the b x can b made of an suita le material which has a low aff inity for the analytes
b ing q antif ied Stainles ste l co t ed with P F f ilm, PMMA an polycarb nate have b en fou d t o b suita le
materials A suita le chamb r can b made from a commer ialy availa le desic at or ca inet with nominal
dimensions of 3 0 mm × 3 0 mm × 340 mm (se Figure 3) This would have an internal volume of 3 dm
3
compared with the airflow volume of 5 dm
3
in 1 min F or non-he t resistant wal materials (e.g PMMA), the
b ck wal of the chamb r an the re r portion of the ro f are protected by a stainles ste l plate f it ed to the
in er surface, the top of the plat e e t en ing 140 mm ac os the chamb r ro f, so as to b resistant o he t an
an flames emanating from the en of the furnace tub
The v lume of the mixing an measur ment chambe ne ds t o be larg e enough t o ac ommodat e the
samplng p int but smal e than the t otal volume of air flowing through the chambe in 1 min
The ro f of the chambe shal be f itt ed with a safety blow-out p nel 7 mm in diamet er, w hich wi l
burs in the event of an ex losion
NOTE 2 This is important or safety re sons
A port a pro imat ely 3 mm in diamet er is pro ided at he b se of the r ar fac of the chambe for the
t es atmosphe e t o be exha ust ed t o wast e
The chambe shal inclu e al the ne es ary samplng an measur ment p int (g s samplng pro es t o
bub le s, et c an p rticulat e filt ers) Measur ment p int ar locat ed awa from the rising plume an
the chambe wal s; these ma be sit ed in any convenient location The o en en of each sample pro e
shal be (3 ± 5) mm from the wal of the mixing an measur ment chambe
NOTE 3 The sampling points are positioned away from the furnace-tub e it plume an chamb r wal s but
can b sited in an convenient location Suita le locations are shown in Figure 3
NOTE 4 A thermocou le (5.3), e ten ing ap ro imately 5 mm into the mixing an me surement chamb r,
can b located as shown in Figure 3, for monitoring of the temperature in the chamb r d ring the tests
5.8 A nal ysis of g ases
This document r q ir s the det ermination of c rtain combus ion g ses t o charact eriz the f ir
con ition The means of g s sampl ng an analy sis shal be those given in ISO 1 7 1 an ISO 1 7 2
The mixing chambe the mocouple shal be locat ed in close pro imity t o the samplng p rt t o ensur
isothe mal samplng conditions
Carb n dio ide an o yg en conc ntrations shal be det ermined b contin ous samplng throughout
the t es These data ar used t o identify and monit or the st eady-s at e burning pe iod and also t o
charact eriz the fir con ition The conc ntration of carb n mono ide shal also be det ermined
contin ously
The o yg en met er shal be ca a le of an ac uracy of a v lume fraction of 0,0 %
The sele tion of t oxic comp nent of the fir ef luent shal folow the a pro riat e hazard as es ment,
such as those set out in ISO 1 34 or ISO 1 5 1
Furthe guidanc isgiven in 1 4
Trang 15Dimensions in milimetr es
Key
2 tub containing p otodetector (se A nne E) 1 secon ary air inlet
3 tub containing lig ht sour ce (se A nne E) 1 port or thermocou le
4 p rg e tub s for p otodetector an lig ht sour ce
(se A nne E)
1 port for tub to sample atmosp er e in furnace tub
for me sur ement of ox yg en concentration
Figure 3 — Dimensions of mixing an me surement chamber
Trang 165.9 Deter mination of smoke aerosols
Smoke ae osols ( old particles an lq id dro let ) shal be b t ch sampled from the mixing an
measur ment chambe through a p rticulat e f ilt er d ring the st eady-s at e pe iod, or p rt the eof
Furthe guidanc isgiven in 1 4
NOTE An e E des rib s optional me surement of the optical density of smok e
5.10 Ex haust system
The sy st em shal be conne t ed t o an efe tive exhaus sy st em, t o ensur the safety of o e at ors an
othe pe sonnel, p rticularly from the t oxic fir ef luent being g ene at ed Howeve , the exhaus sy st em
shal not be conne t ed in such a wa that it draw s air through the a paratus When the primary air
inlet is r mo ed, with the exhaus sy st em at normal o e ating spe d, an se ondary air is not flowing,
o se v ble q antities of air shal not be drawn int o the furnac tube
NOTE Airflow direction can e sily b o served using a jos -stick Jos -sticks can b used t o verify that
smoke is not drawn into the mouth of the furnace, that here is no le ka e at he glan on the mixing chamb r
an t o ensure that an e trane us ef luents wil b drawn into the ho d
6 A ir suppl es
6.1 Pr imar y and sec ondary air suppl es
The primary an se on ary air sup les t o the a p ratus shal be clean an fr e from ex ces ive
mois ur The wat er cont ent an / r the r lative h midity of the air shal be r p rt ed The flow s r fe t o
a pr s ur of 1 1 3 5 Pa an a t empe atur of 2 °C
NOTE 1 Compres ed air from a cy lin er, or compres ed air fre from water an oil, an pas ed through a
carb n trap an silica g l, has b en fou d to b suita le
The primary air shal be introd c d through the closur at the input en of the furnac tube
The se on ary air shal be introd c d int o the mixing an measur ment chambe using piping of
int ernal diamet er (3,5 ± 1) mm, p s ing through the wal of the mixing an measur ment chambe
an en ing (7 ± 5) mm a o e, an in lne with, the en of the furnac tube, an p inting upwards at
an angle of a pro imat ely 45° The se on ary air sup ly int er ept the rising plume t o faci tat e the
eff icient mixing of the t es atmosphe e
NOTE 2 This system wil give g od mixing of the furnace ef luent an the secon ary air an eliminates the
ne d for a mechanical stir ing device
Both the primary and se on ary airflow s shal be del ve ed at a cons ant, pr det ermined rat e, at
p sitive pr s ur an monit or d using in-l ne flow met ers or mas flow controle s Airflow s shal be
calbrat ed at the point of entry t o the chambe
A cor e tion for b ck pr s ur at hein-l ne flow met ers ma be ne es ary
The primary airflow is set t o pro ide the desir d combus ion con itions an the se on ary airflow
shal be adjust ed t o pro ide a t otal airflow through the mixing an measur ment chambe of
6.2 Pr imar y airflow cal bration
Befor t es ing commenc s, the in-lne flow set ing devic (flow met er or mas flow controle ) shal be
calbrat ed for airflow s from 2 dm
t o an ac uracy of 1 % using a bub le met er,
or suita le sup lementary flow met er with no entry or exit r s rictions, with a ma imum rang e of
Trang 17for highe flow s, t o ensur the
cor e t flow of primary airflow through the furnac tube
NOTE When ne dle valves have b en f it ed in-line t o flow meter , these have b en fou d t o ex ert a signif icant
influence on the airflow, even when ful y open
A bor d rub e bu g inse t ed int o the furnac tube at the mixing chambe en , f itt ed with a tube of
int ernal diamet er at leas a fact or of 1,5 larg er than the int ernal diamet er of the primary air inlet tube,
an of length no mor than 1 m, shal be used t o det ermine the primary airflow using this calbration
proc d r , with the drive me hanism in o e ation
6.3 S c ondary air flow cal bration
The se on ary air inlet tube shal be discon e t ed from the chambe Using a tube of gr at er diamet er
than that at the chambe entry, for al conne tions, measur the se on ary airflow o e a rang e from
t o an ac uracy of 1% using an a pro riat e method
NOTE A simple method is to use a larg b re, calibrat ed, 5 dm
3
∙min
−1
rang flow meter with no entry or
e it restrictions (i.e no u per or lower valves) an check me sured a ainst in icated flows on the in-line flow
met er or mas flow controler
6.4 Overal c onfirmation
The a p ratus shal be set up with the furnac of, an the primary air sup ly con e t ed t o a nitrog en
supply Using a primary nitrog en flow of 1 dm
o y g en v lume fraction in the mixing chambe shal be measur d u ti s a le, an then r corded o e a
pe iod of 5 min The measur d averag e o y g en depletion should be (0,041 9 ± 0,0 05)
F or ex mple, if the o y g en met er r ads (1 ,7 ± 0,0 ) %-O
2then this conformation c it erion has be n
met be ausethe v lume fraction of o yg en depletion is 0,2 9 5 −(0,1 7 5 ± 0,0 0 5)= (0,042 ± 0,0 0 5)
In orde t o con rm othe se on ary airflow s, car y out he folowing measur ment :
— The se on ary airflow shal then be inc eased t o 45 dm
In orde t o con rm a lowe primary airflow, car y out he folowing measur ment:
— The primary nitrog en flow shal be set t o 3,0 dm
The measur d a e ag e o yg en depletion should be (0,0 2 6± 0,00 5)
If the r sult is out ide these l mit , the primary an se on ary flow met ers shal be r calbrat ed and
the proc d r isr peat ed u ti conf irmation is o tained
7 Establ shment offurnac e temperatur e and set ing of furnac e temperatur e
The e ar two s ag es inclu ed in the t empe atur s an ardization The f irs s ag e is t o es a lsh that the
t empe atur prof ile (chang e of t empe atur with dis anc through the furnac tube) of the p rticular
furnac t o be used is suita le; the se on s ag e is t o det ermine the t empe atur set ing ne ded for the
p rticular t es run con ition t o be car ied out
Trang 187.2 Establ shing furnac e temperature profi e todetermine furnace suitabi ity
S t up the furnac , with an empty q artz furnac tube in plac , un e s atic con itions ( i.e with no
airflow through the furnac tube) Close the furnac tube at one en with a bung t o pr vent airflow
through the furnac an set the furnac t empe atur control e t o 6 0 °C Introd c the calbrat ed
the mocouple (5.3) int o the c ntr of the q artz furnac tube, with the tip of the the mocouple within a
1 mm radius of the c ntr of the q artz furnac tube
NOTE A suita le su port or the thermocou le is shown in Figure 4
Key
1 position of thermocou le su ports inside furnace tub to position thermocou le in centr e of tub
Figure 4 — W ire thermoco ple sup ort rings alowing thermoco ple to mo e alo g in required
positio
Alow the furnac t o r ach eq i ibrium Then measur the t empe atur profile along the furnac tube
b r cording the t empe atur at int erv ls of 2 mm t o f in the point of ma imum t empe atur This
should be near the c ntr of the furnac an the ma imum t empe atur should be (6 0 ± 1 ) °C If the
ma imum t empe atur is out ide this rang e, adjus the furnac t empe atur controle t o bring the
ma imum t empe atur int o thisrang e
In many cases, it ma be pr fe a le t o use the b at drive me hanism at normal adv nc rat e t o also
drive the the mocouple int o the furnac t o r cord the t empe atur prof ile, as a function of p sition in
the furnac
From the r sult o tained, det ermine the location of the point of ma imum t empe atur an r cord the
tempe atur at that p int Make furthe measur ment at int erv ls of 2 mm on each side of the p int
of ma imum t empe atur , u ti p int ar r ached at w hich the t empe atur de r ase r lative t o the
ma imum t empe atur ex ce ds 1 0 °C F or the furnac t o be ac epta le, these point shal le betwe n
1 5 mm an 2 0mm from the location of the p int of ma imum t empe atur
7.3 S t ing the temperature for an indi vidual test run c ondition
The ma imum t empe atur for an in ivid al t es ru con ition shal be det ermined u de airflow
con itions ( T
ru
), with the q artz furnac tube in plac in the tubular furnac an primary air flowing
through the q artz furnac tube The calbrat ed the mocouple shal be plac d (5.3) in the q artz furnac
tube as desc ibed in 7.2 an alowed t o eq i ibrat e Onc a primary airflow has be n es a l shed, the
point of ma imum t empe atur mo es downs r am r lative t o it location u de s atic con itions
In orde t o compensat e for this shif, p sition the the mocouple tip (7 ± 1 ) mm downs r am of the
point of ma imum t empe atur es a lshed un e s atic conditions (det ermined in 7.2) This position
minimiz s the t empe atur deviation for flow rat es of up t o 2 dm
Trang 19es a lshed, the furnac t empe atur controle shal be adjust ed u ti a t empe atur within ± °C of
the desir d v lue for T
ru
is o tained
NOTE It is neces ary to specify the furnace con itions for the t est The con itions given a ove are b sed
on e perimental work using ty ical commer ial y availa le furnaces 5 0mm to 60 mm long If the furnace hot
zone is to short hen the test specimen an decomposition prod cts might not b he ted for a suff icient ime Hot
zones long r than 60 mm are les likely to present pro lems, but it is pos ible that the long r period for which
the test specimen an decomposition prod cts are he t ed could result in smal diferences in the combustion
prod ct yields T e a ove has b en fou d to b satisfactory in use
8 Test specimen preparation
8.1 Test specimen form
The t es spe imen shal be in the form of eithe
a) gran les or pel et , or
b) a rod or othe contin ous mat erial pro ided st eady-s at e conditions can be achieved (1 3)
Detaisof the t es spe imen an it form shal be inclu ed in the t es r port se Clause 1 )
8.2 Combustible loading
The t es spe imen shal be u iformly dis ribut ed along the length of the combus ion bo t, so that a
cons ant low of de omposition prod ct is prod c d as the t es spe imen p s es through the furnac
The spe imen combus ible lo ding shal be a pro imat ely 2 mg⋅mm
can be so bulky that they r s rict the
flow of air through the furnac tube at a spe imen lo ding of 2 mg⋅mm
−
To o e come this pro lem,
it is ac epta le t o r d c the spe imen lo ding an inc ease the combus ion b at adv nc rat e t o
compensat e (5.6)
F or mat erials w hich contain an ine t matrix or f ile s w hich do not form part of the combus ible mas ,
the mas lo ding of mat erial in the t es spe imen ma ne d t o be inc eased t o compensat e, ac ording t o
Clause 9
8.3 Specimen c onditioning
Befor the t es , spe imens shal be con itioned t o cons ant mas at a t empe atur of (2 ± 2) °C an a
r lative h midity of (5 ± 5) %
Cons ant mas is conside ed t o be r ached w hen two suc es ive weighing o e ations, car ied out at an
int erv l of 24 h, do not dife b mor than 0,1 % of the mas of the t es spe imen or 0,1 g, w hicheve is
the gr at er
Mat erials such as p ly mides, w hich r q ir mor than 1 we k in a conditioning atmosphe e t o r ach
cons ant mas , ma be t est ed aft er con itioning in ac ordanc with ISO 2 1 This pe iod shal be not
les than 1 we k and shal be desc ibed in the t es r p rt
9 Selection oftest dec omposition c onditions
9.1 S lection of dec omposition c onditions for fire hazard anal ysis or fir e safety
eng ine ring
Tes spe imens shal be de omp sed or combust ed un e one or mor of the t es conditions spe ified in
9.2 t o 9.5 for the r q ir d fir s ag es
Trang 20The v rious f ir s ag es ar def ined in ISO 1 7 6:2 1 , Ta le 1 [1 ), 2, 3 ) an 3 )] F or s ag e 2, the
proc d r pro ides an eq iv lenc ratio, Φ, of ≤ ,7 F or s ag es 3 )an 3 ), the proc d r pro idesa Φ
of 2,0 ± 0,2
F or mat erials of un nown de omposition beha iour, pr lminary t es ru s shal be car ied out t o
det ermine the t es con itions ac ording t o the proc d r s of Clause 1 C rbon dio ide an o y g en
conc ntrations, an the a e ag e mas los , shal be measur d in orde t o es a lsh the combus ible
comp nent of the t es mat erial and det ermine the a pro riat e spe imen mas lo ding as spe ified in
9.2 t o 9.5 G idanc on the sele tion of ad itional de omp sition con itionsis pr sent ed in Annex A
NOTE 1 A wel-ventilated t est with a T
ru
of 9 0 °C ac ording t o c) in An e A can b used to det ermine the
combustible content of a mat erial with u k own composition
A t es run is only v ld if the sele t ed st eady-s at e con itions (1 3) ar maintained for a pe iod of at
leas 5min d ring the t es If ignition oc urs d ring a non-flaming ru , or fai s t o oc ur d ring a flaming
ru , then the furnac t empe atur shal be raised or lower d in 2 °Cst eps u ti the r q ir d beha iour
is o tained A new t es ru shal then be car ied out with a fr sh t es spe imen F or flaming beha iour,
it is also ne es ary t o ensur that the cor e t primary airflows ar used, asspe ified in 9.3, 9.4 an 9.5
NOTE 2 The eq ivalence ratio, ϕ, can b calculated from the avera e mas los of combustible efluent from
the test specimen, in mil igrams per min te (mg⋅min
−1
), divided by the mas flow rate of o y gen in the primary
air, in mil igrams per min te (mg⋅min
−1
), divided by the stoichiometric fuel mas t o o y gen mas ratio for the
material u der test.S e worked e ample in An e A
9.2 Stag e 1b): ox idati ve pyrol ysis from ex ter nall y appl ed radiation
Plac a t es -spe imen combus ible lo ding in the combus ion b at t o pro ide a mas fe d rat e of
Complet e a t es ru as desc ibed in the proc d r in 1 2
If flaming de omp sition oc urs d ring therun, r peat at t empe atur s pro r s ively 2 °C lowe u ti
contin ous, non-flaming de omp sition is o tained throughout the st eady-s at e pe iod
9.3 Stag e 2: wel -venti ated flaming
Plac a t es -spe imen combus ible lo ding in the combus ion b at t o pro ide a mas fe d rat e of
Complet e a t es ru as desc ibed in the proc d r in 1 2
From the a e ag e v lume fraction of o yg en in the mixing an measur ment chambe , M
an the measur d o yg en depletion, D
O
2, wi l be 10/5 × 0,2 9 5= 0,041 9
When ϕ = 0,7 , D =0,03 4 0,7 ×0,0419
Trang 21£ an ≥0,0 1 0, then ϕ wi l be ≤ ,7 an ≥ ,5 The ru the efor me t the c it eria for
wel-ventiat ed flaming (ϕ ≤ 0,7 ) A lowe l mit of ϕ = 0,5 is also spe ified be ause, below this, the
combus ible fuel cont ent is t oo low t o o tain r la le data
D
O, eithe b r d cing the combus ible lo ding, or b r d cing the b at adv nc rat e
< and ≥ ,0 5 0, then ϕ < 0,5 an ≥ ,3 an the combus ible fuel cont ent is t oo low t o
o tain r l a le data R epeat he ru , inc easing the spe imen mas lo ding b a fact or of 1,5
< , then ϕ < 0,3 an the combus ible fuel cont ent is t oo low t o o tain r la le data
R epeat the run inc easing the spe imen mas lo ding b a fact or of 2
If flaming de omp sition does not oc ur or is int ermitt ent d ring the ru , r peat at t empe atur s
pro r s ively 2 °C highe , u ti contin ous flaming de omp sition is o tained throughout he st
eady-s at e pe iod If contin ous flaming can ot be o tained, this shal be r p rt ed, t og ethe with the
ma imum furnac t empe atur inves ig t ed
In each case, only data calculat ed from the ac epta le run shal be desc ibed as r pr senting wel
-ventiat ed flaming
NOTE A suita le value of D
O2can also b o tained by set ing the furnace t emperature to o tain a T
ru
of
9 0 °C (se An e A)
9.4 Stag e 3a): smal vitiated fir es in closed or poor l y venti ated c ompartments
Use the same t es spe imen mat erial, lo ding an b at adv nc rat e as in 9.3 in orde t o o tain the
samespe imen fe d rat e
S t he furnac t empe atur t o o tain a T
as desc ibed in the proc d r in 1 2
Calculat e the primary airflow rat e ( P )for the 3 )t es as folow s:
is derived from the total airflow, the volume fraction of o y gen in the air
su ply an the targ t value of ϕ, as fol ows, taking into ac ou t an avera e combustion eff iciency fraction of 0,9
Trang 22NOTE 2 T e fact or of 0,9 has b en shown to compensate for les than complet e mixing of fuel an o idizer in
the furnace tub
dife ent from this should be taken int o ac ount and the fact or r calculat ed
NOTE 3 T e minimum primary airflow of 3,2 dm
3
·min
−1
is to ensure that the targ t con ition of ϕ = 2,0± 0,2 is
met, even when wel -ventilated combustion is incomplet e F or e ample, flame in ibition by halo ens can red ce
the combustion eff iciency in wel -ventilat ed con itions le ding t o an incor ectly low calculated primary airflow
If flaming de omp sition does not oc ur or is int ermitt ent d ring the run, the run shal be r peat ed
at t empe atur s pro r s ively 2 °C highe , u ti contin ous flaming de omp sition is o tained
throughout the st eady-s at e pe iod If contin ous flaming can ot be o tained, this shal be r p rt ed,
t og ethe with thema imum t empe atur inves ig t ed
In each case, only data calculat ed from the ac epta le ru shal be desc ibed as r pr senting u
der-ventiat ed flaming
9.5 Stag e 3b): post-flashover fires in open c ompar tments
The proc d r is the same as that spe if ied in 9.4, ex cept that the furnac tempe atur is set at a T
ru
of 8 5 °C
10 Proc edure
10.1 S fety c onsiderations
WARNING — So that suitable precautions are taken to safe uard he lth, the attention of al
co cerned in fire tests is drawn to the pos ibi ity that toxic or harmful g ses can be ev lved
during ex osure of test specimens
The t es proc d r s inv lve high t empe atur s an combus ion proc s es The efor , hazards can exis
such as burns or the ignition of flamma le g ses, extraneous o je t or clothing The o e at or shal use
prot ective glo es for inse tion an r mo al of t es spe imens Neithe the furnac nor the as ociat ed
fixtur s shal be t ouched w hie hot ex cept with the use of prot ective glo es The exhaus sy st em of the
a paratusshal be che ked for pro e o e ation an shal discharg e int o a buiding exhaus sy st em with
adeq at e ca acity The p s ibi ity of the ac umulation of flamma le f ir efluent in the mixing chambe
w hich then ignit es causing an ex losion can ot t otaly be discou t ed, an it is the efor es ential that
eyeprot ection be worn
When the furnac ishot, the chambe wals shal only be cleaned with wat er-b sed fluids Cleaning the
chambe wal s with flamma le solvent-b sed fluids should only becar ied out w hen the furnac is cold
10.2 Dec omposition of the test specimen
The furnac tubean combus ion b at shal be clean befor each t es (5.5, Not e 4 ) The mixing chambe
shal be fr e of any lo se mat erial befor each t es A blank t es ru car ied out befor each se ies of
t es s can be used t o con rm thecleanl nes of the a p ratus
S t up the tubular furnac at the spe if ied t empe atur an primary airflow rat e in ac ordanc with
Thesampl ng an measur ment eq ipment shal becalbrat ed daiy
Introd c the combus ion b at containing a t es spe imen of k own mas , pr p r d in ac ordanc with
Clause 8, int o the q artz furnac tube with the front en of the b at jus out ide the air inlet en of
Trang 23Begin contin ous samplng from the chambe through the g s analy se s (carb n dio ide, carb n
mono ide an o yg en) Start r cording the data from these an from the smoke density monit or if
fitt ed ( e An ex E)
Start the t es ru b swit ching on the b at drive me hanism t o introd c the combus ion b at
containing the t es spe imen int o the furnac at an adv nc rat e of 40 mm ⋅min
In this case, it ma be ne es ary t o chang e the spe imen mas an airflow rat es t o
maintain a cons ant fuel-mas / irflow ratio (5.6an 8.2)
R egular visual o se v tion of the spe imen inside the furnac tube shal be made t o det ermine w hen
ignition oc urs, that flaming is contin ous d ring flaming de omp sition t es s an that flaming does
not oc ur d ring non-flaming de omp sition t es s
NOTE 1 A convex mir or at the primary air inlet en of the furnace tub has b en fou d useful for this
The f ir condition can also be ve ified from the g s analysis w he e flaming wi be in icat ed b
r latively high CO
2conc ntrations an yields
The signals from the g s analy se s (carb n dio ide, carb n mono ide, o yg en an the smoke density
monit or if f itt ed) shal be r corded throughout the ru an the signals o se ved d ring the early
s ag es of the ru When these ha e r ached a pro imat ely cons ant levels, then dynamic st eady-s at e
con itions ha e be n achieved R ecord the time an begin any bat ch sampl ng from the chambe aft er
this point The data lo ging int erv l shal beno long er than 1 s
Develo ment of st eady-s at e con itions: During the firs few min t es of a 2 -min ru , the leading edg e
of the spe imen be ome pro r s ively hott er u ti a s a le flame is es a l shed from a pro imat ely
4 min Aft er a furthe 2 min, d ring w hich eq i ibrium con itions ar es a lshed in the mixing
chambe , st eady-s at e con itions ar es a l shed for non-char forming mat erials and maintained
for the r main e of the ru F or char-forming mat erials, a furthe few min t es ar r q ir d for the
char de omposition rat e t o r ach eq i brium F or al mat erials, inclu ing char forme s, st eady-s at e
con itions ha e be n fou d t o exis from a pro imat ely 1 min aft er the s art of the t es ru Bat ch
samplng can then be s art ed at any time betwe n 1 min an 1 min t o pro ide a sampl ng pe iod of at
leas 5min F or r sult calculations aft er a ru , a default st eady-s at e pe iod from 1 min t o 2 min ma
be used, but inc eased ac uracy can be o tained b r trospe tive ex mination of the data w hich can
ext en the pe iod used for calculation of st eady-s at e g s conc ntrations t o earl e times an lengthen
the st eady-s at e pe iod w hen p s ible
NOTE 2 F or man materials, initial pe ks in CO
2
an CO are o served ne r the start of the ru as the flame
sta ilizes, afer which a period of st ead burning is g eneral y o served for the remain er of the ru u to 2 min
If the ru is prolong d b yon the specif ied period, or a short er than specif ied test specimen is used,so that uel
is consumed over the entire length of the combustion b at, then ir e ularities can oc ur t owards the en of the
ru , so that he period of st ead burning is then b tween these two re ions
Contin e t o o se ve the t es spe imen and signals from the g s monit ors The de omposition con itions
shal r main a pro imat ely st eady for a minimum of 5 min, but long er if p s ible, t o ena le the spe imen
de omp sition beha iour and t oxic prod ct yields t o be charact eriz d Al measur d paramet er data
shal be used t o o tain a e ag e v lues o e this st eady-s at e pe iod
When the up-s r am en of the combus ion b at ent ers the tubular furnac , the run is complet ed
Swit ch of the b at drive me hanism an g s samplng sy st ems, pumps an bub le s Immediat ely
with raw the b at t o it s arting p sition in the furnac tube an extinguish any flame b t emporariy
int er upting the primary airflow
When the t es spe imen r sid e an combus ion b at ha e co led, r mo e them from the q artz
furnac tube, st or in a co l, s a le atmosphe e an r weigh w hen the b at and cont ent ha e r ached
cons ant mas , ac ording t o 1 4.3
Trang 2410.3 Stead y-state period
The st eady-s at e pe iod shal be used as the b sis for calculating r sult If flaming combus ion can ot
be o tained, or w he e only int ermitt ent laming oc urs, this shal be r p rt ed The r sult of the t es s
ar not v ld in t erms of the spe if ied f ir s ag es 1b), 2, 3a) or 3 ) if st eady-s at e con itions as def ined
below ar not o tained for a minimum of 5 min If flaming oc urs in the mixing chambe d ring the
st eady-s at e pe iod, this inv ldat es the q antif ication of the eq iv lenc ratio an the ru should
be r peat ed; if ne es ary, the primary airflow shal be inc eased, g ene ating data cor esp nding t o a
sl ghtly lower eq iv lenc ratio
During dynamic st eady-s at e con itions, the v lume fractions of carb n dio ide an o y g en depletion
in the mixing an measur ment chambe shal r main a pro imat ely cons ant, such that b th
a) for any long -t erm tr n , the a e ag e rat e of chang e of v lume fraction divided b the averag e v lue
of the v lume fraction over the 5-min pe iod shal be les than ±0,0 0 min
−
;
b) for any short-t erm fluctuations, the s an ard deviation of the v lume fraction divided b the
a e ag e v lue of the v lume fraction, o e the 5-min pe iod shal be les than 0,2
Carb n mono ide (CO) an smoke conc ntrations ma be somew hat mor v ria le in some cases If
larg er fluctuations oc ur, then this shal be r port ed If st eady-s at e con itions cannot be maintained
for at leas 5 min, then it is ne es ary t o use a long er furnac combus ion b at or r d c the rat e of
introd ction of the combus ion b at t o inc ease the d ration of the ru A 2 -min run has be n fou d t o
pro ide a st eady-s at e pe iod of at leas 1 min d ration for mos mat erials If this is not achiev ble in
r plcat e ru s, the o se ved v riation shal be inclu ed in the r p rt
Whe e diff iculties ar encou t er d in o taining st eady flaming conditions, these can oft en be o e come
b v rying the fuel lo d or de omp sition t empe atur If ignition oc urs d ring a non-flaming ru , or
fai s t o oc ur d ring a flaming ru , then the furnac t empe atur shal be raised or lowe ed in 2 °C
st eps u ti the r q ir d beha iour is o tained A new t es ru shal then be car ied out with a fr sh
t es spe imen F or flaming beha iour, it is also ne es ary t o ensur that the primary airflow rat es ar
cor e t for one of the thr e s at es: wel-venti at ed flaming, smal un er-ventiat ed or p s -flasho e
un er-ventiat ed The e shal be ex ces o y g en d ring wel -venti at ed flaming an fuel-rich con itions
for un er-ventiat ed flaming This is achieved b folowing the proc d r desc ibed in Clause 9 The
burning beha iour of c rtain mat erials is so depen ent on the venti ation con ition that the r sult
from the wel -venti at ed t es do not al ow ac urat e pr diction of the degr e of combus ion in u
der-ventiat ed con itions ( e 9.3) In these cir ums anc s, it is ne es ary t o r peat an u der-ventiat ed t es
with a smale primary airflow in orde t o satis y the eq iv lenc ratio c it erion ( i.e ϕ = 2,0 ± 0,2) If
this proc d r fais t o satis y the eq iv lenc ratio c it erion, this shal be r p rted
10.4 S mpl ng and anal ysis of fire efluent
10.4.1 General
The conc ntrations of al ef luent component (g ses an r spira le ae osols) that contribut e
significantly t o the computation of the t oxic hazard shal be measur d d ring the st eady-s at e t es
pe iod The methods ofanaly sis shal conform t o the spe ifications in ISO 1 7 1 an ISO 1 7 2, an as
defined below The in ivid al comp nent ar identif ied in the a pro riat e hazard as es ment ( uch
Trang 25pe iod The t otal extract ed flow shal not ex ce d 5 dm
3
·min
−
If additional ef luent is r q ir d, it shal
be taken from the exhaus p rt of the mixing chambe , close t o the chambe ISO 1 7 1 and ISO 1 7 2
pro ide information on the samplng of f ir efluent
10.4.2.2 S mpl ng and anal ysis of O
2, CO and CO
2shal pas through
a suita le drying ag ent an a smoke f iltration sy st em en ro te t o the a pro riat e analy se s The
conc ntrations of these g ses shal be det ermined contin ously
NOTE 1 Details of a suita le f iltration an drying system an analyser for these are given in ISO 56 0-1
[7]
NOTE 2 T e results for o y gen, carb n mono ide an carb n dio ide concentrations are relative to dry g s,
af er water vapour has b en removed
10.4.2.3 S mpl ng and anal ysis of acid gases
The folowing acid g ses shal be det ermined, unles measur ment has be n de med u ne es ary b
elemental analy sis or cita le know ledg e
HCN, HCl, HBr, HF, NO
x
an SO
2
ma be det ermined eithe b samplng through bub le s as desc ibed
below, folowed b analytical proc d r s desc ibed in ISO 1 7 1, or b g s phase F ourie trans orm
infrar d analy sis (FTIR) desc ibed in ISO 1 7 2
Pas a contin ous sample of the f ir ef luent at an a pro riat e flow rat e through two g s bub le s
plac d in se ies, each containing an a pro riat e v lume of the a pro riat e a sorbent The samplng
shal be car ied out at a cons ant rat e for a minimum of 5 min d ring the pe iod for w hich dynamic
st eady-s at e con itionsar maintained
NOTE 1 Calibrat e the sampling flow rate using a bub le meter (des rib d in ISO 1 70 )
NOTE 2 A flow rate of 1dm
3
⋅min
−
pas ing through two 2 0 ml Dres helb t les f it ed with sintered glas of
porosity zero,e ch containing 1 0 ml of a sorbing solution, has b en fou d to b efective
0,1 M aq eous sodium hydro ide solution has be n fou d suita le for the acid g ses l st ed a o e, ex cept
t o be det ermined b a dedicat ed method Detais ar given in ISO 1 7 1
10.4.2.4 S mpl ng and anal ysis of or ganic gases
The org nic fraction of the ef luent contains many ir itant spe ies A n mbe of methods ar suita le
for q antifying the org nic fraction of the ef luent an , if a pro riat e, the conc ntrations an yields of
in ivid al org nic compoun s The proc d r s ar desc ibed in ISO 1 7 1an ISO 1 7 2
The minimum r q ir ment is for an es imat e of the t otal org nic cont ent of the ef luent
One of the folowing methods shal be used t o measur the org nic cont ent of the ef luent
a) A t otal hydrocarbon analy se shal be used t o o tain an a pro imat e es imat e of the t otal
hydrocarb n cont ent of the efluent
NOT 1 A t otal hydrocarb n analysis do s not ena le an ac urate me sure of the potency of the org nic
b cause the org nic fraction of the smoke contains man ir itant species T e ir itant potency of
non-o idized org nic is relatively low compared with that of the partial y o idized compou ds, but the sum of
the lat er concentrations is g neral y much smaler than the sum of the former concentrations Overal, a
high org nic content is as ociat ed with higher levels of ir itancy Crucialy, this determination provides the
data t o q antify the fraction of u burnt an partial y burnt carb n an therefore alows carb n b lances to
b esta lished
NOT 2 A limitation of this method is that, since the identities of the org nic compou ds in the ef luent
are u k own, the ap ropriat e response factor are also u k own
Trang 26b) The fraction of carb n in the ef luent in the form of org nic carb n shal bedet ermined b o idizing
a sample of the ef luent from the mixing an measur ment chambe an measuring the CO
2
conc ntration The org nic fraction shal then be det ermined b comp ring the CO
2conc ntration
in the o idiz d sample with the conc ntrations of CO
2, CO an so t p rticulat es in the mixing an
measur ment chambe in ac ordanc with 1 4
c) F or t es spe imens with a k own comp sition, the org nic fraction shal be es imat ed a pro imat ely
from the CO
2, CO an so t p rticulat es in the mixing an measur ment chambe , an thees imat ed
carbon-mas -los conc ntration from the t es spe imen
d) Dir ct measur ment shal be made of a rang e of in ivid al org nic spe ies This ma inclu e
ir itant (e.g ac olein an formaldehyde) an othe t oxic org nic spe ies (e.g benz ne, p lycyclc
aromatic hydrocarb ns)
10.4.2.5 S mpl ng of a rosols and particulates
Smoke ae osols ( old particles an lq id dro lets) ar b t ch sampled from the mixing an measur ment
chambe through a p rticulat e filt er d ring the st eady-s at e pe iod, or p rt the eof The f ir ef luent in
the mixing an measur ment chambe shal be sampled contin ously through a particulat e f ilt er at an
a pro riat e flow rat e using the same proc d r asin 1 4.2.3
A sampl ng pe iod of 5 min at a flow of 1,0 dm
3
·min
−
is r commen ed
The filt er shal be weighed befor sampl ng and within 1 min aft er samplng, an also aft er
con itioning t o cons ant mas in a desic at or charg ed with a drying ag ent (t o isolat e the efe t of
con ensed mois ur ), in orde t o calculat e the mas of p rticulat es dep sit ed
NOTE 1 A glas mic of ibre f ilter 0,26 mm thick with a 1,6 µm particle retention characteristic an a diameter
of 37 mm has b en fou d t o b suita le
NOTE 2 For ex ces ively so ty samples, a shorter sampling period or lower flow can b used t o ensure
consist ent low through the f ilt er
NOTE 3 It is not pos ible t o design true isokinetic sampling for the mixing an me surement chamb r without
characterization of the flow en ironment at he sample point However, as the cont ent in chamb r is wel mix ed
an the flow is rather slow, anisokinetic, sampling is e pected t o have very lit le impact on the total so t yield
me sured Guidance on sampling for a rosol me surements, to ensure ne ligible anisokinetic sampling er or is
provided in ISO 2 9 4:2 1 , 5.6.1)
[8]
10.4.3 Deter minatio of the mas of the specimen residue
A t the en of the run, w hen the combus ion b at has co led suff iciently, it shal be r mo ed from the
entranc of the furnac tube an st or d in a co l, s a le atmosphe e t o achieve cons ant mas
Inspe t the bo t for the pr senc of r sid e in the f irs 400 mm If r sid e is pr sent in this r gion
(w hich ma be ine t mat erial or char), mark the bo t at 40 mm from the front en , car fuly r mo e
the portion of r sid e contained the ein, weigh it an r cord it mas R ecord the length as 400 mm
an calculat e themas of r sid e pe mi lmetr (mg·mm
−
) If the e is no visible r sid e in this r gion,
r cord the length of r sid e as 40 mm an the mas of r sid e pe mi imetr as z ro Do not inclu e
othe r sid e or u afe t ed mat erial bey n 40 mm Do not inclu e so t dep sit at the front en of
the b at, asthese wi ha e be n q antified ac ording t o 1 4.2.5
NOTE T is represents the mas of resid e per mil imetre o tained u der ste d -state con itions (m
r s)an
is req ired in 1 2.2 to calculate the avera e mas -los concentration in the mixing an me surement chamb r
d ring the ste d -state period
10.4.4 A mbient c onditio s
The t empe atur an pr s ur of the sur ou dings shal be r corded so that hey can be used t o a ply
Trang 2710.5 Val dity oftest run
A t es run is only v ld if the sele t ed st eady-s at e burning con itions ( e Clause 9 an 1 3) ar
maintained for a pe iod of at leas 5 min d ring the t es If ignition oc urs d ring a non-flaming run,
or fai s t o oc ur d ring a flaming ru , then the furnac t empe atur shal be raised or lowe ed in 2 °C
st eps u ti the r q ir d beha iour is o tained A new t es ru shal then be car ied out with a fr sh
t es spe imen F or flaming beha iour, it is also ne es ary t o ensur that the primary airflow rat es ar
cor e t as spe ified in 9.3, 9.4 and 9.5
11 Calculations
11.1 General
The calculat ed v lues ar a e ag es o e the d ration of the st eady-s at e p rt of the t es This pe iod is
def ined in t erms of the conc ntrations of carb n dio ide, carb n mono ide an o y g en (1 3) St eady
consumption of O
2
an prod ction of CO
2
is taken t o be in icative of st eady prod ction of al v lati e
combus ion prod ct F or contin ously monit or d paramet ers, the mean, s an ard deviation an
s an ard e ror shal becalculat ed from the data lo g ed at pro r s ive int erv lsthroughout the st
eady-s at e pe iod
The r sult shal be calculat ed t o two signif icant f igur s
11.2 Mas -char g e c onc entration and mas - os c onc entration
11.2.1 Mas -char g e c onc entratio
Calculat e the mas -charg e conc ntration, C
11.2.2 Mas -os c onc entration
Calculat e the mas -los conc ntration as folow s
a) Calculat e the mas los pe u it length, m
los, in mi lgrams pe mi imetr (mg⋅mm
Trang 28b) Calculat e the mas -los rat e,
m
los, in mi lgrams pe min t e (mg⋅min
NOTE Mas -los concentration calculat ed in this way from the mas lo ding an the resid e mas lo ding
has b en shown to b in a re ment with mas -los concentration d ring the ste d -state period calculated from
the contin ously me sured prod cts for b th non-char ing an char forming materials
ar oft en ex r s ed as g·g
−
or kg·kg
−
for clarity), of each efluent comp nent (an for contin ously
measur d p ramet ers their s an ard deviations an s an ard e rors)using F ormulae ( 8) t o (1 ):
Y
m.charg
= (M/V ) ×(F
v/C
M is the molar mas of the comp nent ;
V is the molar v lume of the comp nent at 2 °C t empe atur an 1 1,3 5k a pr s ur ,
as uming that it beha es as an ideal g s (=0,0 4 0 5 m