INTERNATIONAL STANDARD ANSI intesnat Ds@ See IS0 301 3 Second edi tion 1 997 09 l 5 Petroleum products Determination of the freezing point of aviation fuels Produi ts p&rol iers D&termination du point[.]
Trang 1STA NDA RD
Seco d e itio
19 7-0 -l 5
Prod its p& rolers - D& termina tion d p int de disp a rition des c ristaux
des ca rbura nts av iation
Refere ce numb r
IS0 3 13: 19 7(E)
Trang 2Foreword
IS0 (the Interna tiona l O rganization f or Stan ardization) is a worldwide
f edera tion of national stan ard b dies (IS0 memb r b dies) T he work of
pre a rin Interna tiona l Stan ard is normaly ca rried out throu h IS0
tec hnic al c ommite s Eac memb r b d interested in a s bjec t for whic h
a tec hnic al c ommite has b en esta ls ed has the rig t to b re resented
on that c ommite Interna tiona l orga nization , governmental an non-
governmental, in la ison with ISO , also ta e pa rt in the work IS0
cola ora tes c losely with the Interna tiona l Elec trotec hnic al Commis ion
(IEC ) on a ll maters of elec trotechnic a l stan ardization
D raf Interna tiona l Stan ard ado ted by the tec hnic al c ommite s a re
circ ula ted to the memb r b dies f or votin Publcation as an Interna tional
S tan ard req ires a prova l by at le st 7 % of the memb r b dies c astin
a v ote
Interna tiona l Stan ard IS0 3 13 was pre ared by T ec hnic al C ommite
ISOR 2 , Petroleum prod c ts an lubricants
This sec on edition c anc els an re laces the f irs t edition (IS0 3 13:19 4)
whic h has b en technicaly revised, in pa rticula r with the inc lu ion of
a nnex A
An ex A forms an integra l pa rt of this Interna tiona l Stan ard
0 IS0 19 7
All rig ts re erved Unle s oth rwis spec ifie , n pa rt of his publc a tio may be repro uc ed
or utiz d in an form or by an mean , elec tro ic or mec hanic al inc lu in ph toc opy in a nd
microfim, with ut permisio in writin fom th publs er
Interna tio a l O rganizatio for Stan ardizatio
Cas po tale 5 l C H-121 Ge eve 2 l Switz rlan
Intern t c enta l 8 is c
x 40 c=c ; a lO O net; p is ; o=is c s; s=c ental
Printe in Switz rlan
Trang 3Petroleum produc ts
WA RNING -
T he u e of this Interna tiona l Stan ard may involve hazardou materia ls, o era tion an
eq ipment T his Interna tional Stan ard do s not purp rt to ad res a ll of the safety pro lems as oc iated
with its u e I is the resp n ibi ty of the u er of this Interna tiona l Stan ard to esta ls a ppro ria te safety
an hea lth prac tic es an determine the a plca bi ty of reg latory lmita tion prior to u e
T his Interna tional Stan ard sp c ifies a proc ed re f or determinin the temp rature b low whic sold hy droc arb n
c ry stals a re present in a via tion turbine fuels or a viation gasolnes
T he folowin stan ard c ontain provision whic h, throu h reference in this tex t, c on titute provision of this
Interna tiona l Stan ard At the time of publc a tion, the edition in ic a ted were va lid Al stan ard a re s bjec t to
revision, an p rties to agre ments b sed on this interna tiona l Stan ard a re enc ouraged to investigate the
p s ibi ty of a plyin the most rec ent edition of the stan ard lsted b low Memb rs of IEC an IS0 maintain
registers of curently vald Interna tiona l Stan ard
IS0 317 :19 8, Petroleum lq id - Man al sampln
IS0 3171 :19 8, Petroleum lq id - Automatic pip lne sampln
3 Definitio s
F or the purp ses of this Interna tiona l Stan ard the folowin definition a ply:
3.1 fre zin p int T he temp rature a t whic h sold hy droc arb n c ry stals, formed on cooln , disa p ar when the
temp ra ture of the test sample is alowed to rise
3.2 crystal zation p int T he temp rature at whic h c ry stals of hy droc arb n f irs t a p a r when the test sample is
cooled
4 Princ iple
T he sample tub , c ontainin the test sample, a stirer, cola r an thermometer, is plac ed in a v ac um flask
containin a coola nt Durin the cooln c y c le the test sample is s tired vigorou ly an ex amined for the formation of
Trang 4c ry stals When c ry stals a re o served, the temp rature is recorded as the crystal zation p int T he jac keted sample
tub is then remov ed from the coolant an the test sample alowed to warm up slowly S tirin c ontin es u ti a ll
cry stals disa p a r, at whic h p int the temp rature is recorded as the fre zin p int
5 R eagents a nd materials
5.1 C oolant
Use one of the folowin lq id sp c ified in 5.1 to 5.1.4 in c ombination with sold c arb n diox ide (5.15) or lq id
nitrogen (5.1.6) u der the sp c ified c on ition only
5.1 Prop n-2-01 [(CH CHOH] c ommerc ial gra de of dry pro a nQ -ol
NOT - Pro an-P-01 is the pref ered lq id for u e as the c oola nt
5.1.2 Ethan l (C 2H,0H) c ommerc ial grade of dry etha nol
5.1.3 Aceto e
(CHsCOCHs) c ommerc ial gra de, provided it do s not le ve a resid e
5.1.4 Methanol (CHsOH) c ommerc ial grade of dry methanol
5.1.5
C arb n diox ide (s old) or “dry ic e”, c ommerc ial grade
WA RNING - Ex tremely c old, - 7 “C L ib rated gases c an c au e s focation
NOT - Mec hanic al refrigera tion is p rmited provided tha t the c oola nt temp rature is in the ran e - 7 “C to - 8 “C
5.1.6 Nitrogen (lq id) c ommerc ial grade Use only when determinin the fre zin p int of avia tion gasolnes, or
if he fre zin p int of the a viation turbine fuel is lower than - 6 “C
WA RNING - Ex tremely c old, - 19 “C L ib ra ted gases c an c au e s foc a tion
5.2 Nitrogen gas or dry a ir, a s p ly of nitrogen gas of low moisture c ontent or dry a ir s a ll b u ed if moisture-
pro f cola r A is uti zed
5.3 Fibreglas , c ommerc ial gra de, for u e in moisture-pro f cola r B
Use one of the folowin :
5.4.1 C alcium s lfate (C aS04), gra nulated an y drou c alc ium s lfate, for u e as a desic c ant in moisture-pro f
cola r B, or to as ist in dry in the nitrogen gas or a ir (5.2) u ed with cola r A
5.4.2 Si c a gel, 1.7 mm, for u e as a desic c ant in moisture-pro f cola r B, or to as ist in dryin the nitrogen gas or
a ir (5.2) u ed with cola r A
Trang 56 App ratu
Se fig re 1
6.1 Ja ck ted sample tub , a double w led, u siv ered v es el, simiar to a Dewar flask; the sp ce b twe n the
ja ck ted sample tub an the outer gla ss jack t b in fi ed, at a tmospheric pres ure, with dry nitrogen or air T he
mouth of the tub s all b closed with a cork sto p r s p ortin the thermometer an c olar throu h whic the
stir r er pa sses
6.2 C olar, a s s own is either fig re 2 or 3, an moisture-pro f to in ib it the in res of moisture into the test
sample
6.3
S tirr er , a bra ss or stainles ste l rod, 1,6 mm in dia meter, b nt into a smo th thre lo p sp iral at the b tom,
NOT - T he stirr er can b mec a nica lly a ctua ted
6.4 V ac um flask, an u siv ered vac um flask of the dimen ion s own in fig re 1 T he ca pa c ity s all b
s fic ient to hold an a deq a te volume of c oola nt (5.1) an p rmit the neces ary de th of immersion of the ja c keted
sa mple tub
6.5
T hermometer, conformin to an ex A
Al gla sswa re s all b clea n an dry b fore u e
7.2 C ol a r
As emble the c olar (6.2) thermometer (6.5) an stir r er (6.3) into the c ork
7 2.1 C ola r typ A, flu h with nitrogen or dry air (5.2) b fore fitin to the ja ck ted sample tub , an throu hout
the entire determina tion
NOT - T he air can b efec tively dried by pa ssin throu h a bsorb nt tub s fi ed with deh dra tin a gents (5 1 an 5.4.2)
7 2.2 C ola r typ B, f il with fibregla ss (5.3) an a s ita b le deh dra tin agent (5.4.1 or 5.4.2) a s s own in fig re 3
T he fib regla ss s a ll b re la ced ev ery fourth test T he deh dra tin a gent s ould b renewed at interv als of not more
tha n 3 month or when a c olour c an e s ows it to b inefec tiv e
7.3 Vac um fla sk
In ert s fic ient co la nt (5.1) to me t the immersion de th req irements s own in fig re 1
Obta in samples in ac orda nce with IS0 317 , IS0 3171 or an eq iv a lent na tiona l sta nda rd
Trang 6Stirer - -
Moisture-p ro f
c olar
-1
Cork stop er
Dime sio s in mi metres
,- Thermometer
Jacete sample tube
o ter tube: 0
ex t 3 m
0 int 2 m
in er tube: 0 ex t 2 m
0 int 18 m
Un ivere v ac um
-0int.?O m in
j/C oolant
-Sold
C a rbo diox id
flas
Fig re 1 -
Ap aratu for determinin the fre zin p int of a viation fuels
Trang 7:
B
I I
/
Dime sio s in mi metres
Inlet for dry a ir
In er into c rk
thro g tube)
F ig re 2 -
Moisture-pro f cola r ty pe A
-Fibre las
-De y dratin a ge t
In er into c rk
-stirer p se
thro g tube)
F ig re 3 -
Moisture-pro f cola r ty pe B
Trang 89 Proc edure
9.1 T ran fer 2 ml + 1 ml of test sample to the c le n an dry jac keted sample tub (6.1) C lose the tub tig t1
with the c ork holdin the s tirer, thermometer an cola r; adju t the thermometer p sition so that its bulb is 10 mm t
15 mm a ov e the c entre of the b tom of the tub
9.2 C lamp the jac keted sample tub so that it ex ten s into the v ac um flask (6.4) c onta inin the coola nt T h
s rfac e of the test sample s a ll b a prox imately 15 mm to 2 mm b low the level of the coola nt Add sold c arb
diox ide (5.1.5) as nec es ary throu hout the test to maintain the c oolant level in the v ac um flask
WA RNING - Do n t ad s ld c arbo diox ide to lq id nitro en
9.3
Exc ept when ma in o servation , stir the test sample c ontin ou ly , mov in the s tirer up an down a t a ra t,
of b twe n one c y c le p r sec on an 1,5 c y c les p r sec on Stir the test sample from to to b tom, ta in c a r!
tha t the stirer lo ps do not ma e c ontac t with the b tom of the jac keted sample tub or travel a ov e the tes
sample’s s rfac e
9.4 Durin the c ooln c y c le examine the test sample for the presenc e of c ry stals Disregard an c lou the
a p ars at a prox imately - 10 “C an do s not inc re se in inten ity as the temp rature is lowered; this is d e t
water Howev er s ould s c h a c lou a p a r, note the o serva tion in the re ort sp c ify in the temp rature whe,
the c lou firs t a p ared an a description of its p rsistenc e
When the forma tion of c ry stals is noted, record the temp rature as the o served crysta llzation p int
NOT S
1 A difu ed, c ool, lg t sourc e is rec ommen ed to as ist in viewin the formation an disa p aranc e of the c ry stals
2 If it b comes dif ficult to v iew the a p aranc e of c ry stals d e to gases relea sed by the c oolant the jac keted sample tub
may b remov ed from the c oolant f or a p riod not exc eedin 10 s If c ry stals a re fou d to have a lre d formed, note thl
temp rature of the sample an alow the sample to warm u ti it is 5 “C warmer than the temp rature when the c ry stals an
se n to disa p ar T he sample tub s ould then b re laced in the c oolant an alowed to cool T he crysta llzation p int ma
then b o serv ed by remov in the sample tub from the c oolant when the temp rature of the sample is slg tly warmer tha l
the noted temp rature
9.5 When the c ry stal za tion p int has b en determined, remov e the jac keted sample tub from the coolant
c ontin e stirin a t a ra te of b twe n one c y c le p r sec on an 1,5 c y c les p r sec on , an alow the test sample tc
warm up slowly O bserv e the test sample an when the c ry stals c ompletely disa p ar, rec ord the temp rature a:
the o served fre zin p int
C orec t the o served fre zin an crysta llzation p ints by a pply in the releva nt thermometer cor ection When tht
o served fre zin or cry sta llza tion p int is b twe n two ca libra tion temp ratures, o ta in the c orection at the
o served temp ra ture by lnea r corela tion R ep rt the corec ted fre zin p int to the ne rest 0,5 “C
T he prec ision of this method, as o tained by statistical ex amination of interla bora tory test res lts, is as folows:
1 l R ep ata i ty , r
T he diferenc e b twe n s cc es iv e test res lts, o ta ined by the same o era tor with the same a p ratu u de
c on tant o era tin c on ition on identical test ma teria l, in the normal an c orect o era tion of the test method
would exc eed the folowin value in only one c ase in twenty
r = 0,8 “C
Trang 91 2 R epro uc ibi ty , R
T he diferenc e b twe n two sin le an in e en ent res lts, o tained by diff erent o erators in diferent la bora tories
on nominaly identica l test materia l, in the normal an corect o era tion of the test method, would exc eed the
folowin value in only one c ase in twenty
R = 2,3 “C
1 T he precision has b en determined ac c ordin to IS0 4 5 ex c ept that the rou din rules hav e not b en a pled in this
in tanc e
2 T he sample matrix on whic h the precision of this stan ard is b sed did not inc lu e a viation ga solne
12 T est re ort
T he test re ort s al c ontain a t lea st the folowin information:
a ) a referenc e to this Internationa l Stan ard;
b) a ll deta ils nec es ary f or the c omplete identifica tion the prod c t tested;
c ) the res lts of the test (se c lau e 10)
d) an devia tion, by agre ment or otherwise, from the proced re sp c ified;
e) the date of the test
Trang 10A nnex A
A.1 Th th rmometer d s rib d in 6.5 sha ll me t th re uireme ts giv n in ta le A 1
Ta le A.1
- Req irements for the thermometer for the determination
of the fre zin p int of a v ia tion fuels
Ra g
- 8 “C to + 2 “C
Im ersio
T otal
Gra uatio s at e ch
0,5 “C
L n er ln s at e ch
1 “C a d 5 “C
Figure a t e ch
5 “C
Exp nsio ch mb r p rmitin h atin to
45 “C
O veral le gth
Stem diameter
6,0 mm to 8,0 mm
Dista ce from b tom of bulb to 0 “C ln
2 0 mm maximum
NOT S
A 1 Th rmometer typ IP 14CIA TM 1 4C me ts th a o e re uireme ts
A.2
T olu n is s ita ble as th a ctua tin lq id
A.3
Th th rmometer s al hav a va lid ca libra tio c rificate
Trang 11ICS 7 160.2
Des riptors: Petole m Pro uc ts, automotive fu ls, avia tio fu ls, te ts, ph sic al te ts, low tempera ture te ts, d terminatio , s ldific atic
point
Pric b s d o 8 pg s