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[.]
IS0 INTERNATIONAL STANDARD 301 ANSI intesnat Ds@See Second edition 997-09-l Petroleum products - Determination of the freezing point of aviation fuels Produits p&roliers - D&termination du point de disparition des cristaux des carburants aviation Reference number IS0 301 3: 997(E) IS0 301 3:1 997(E) Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies) The work of preparing International Standards is normally carried out through IS0 technical committees Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee International organizations, governmental and nongovernmental, in liaison with ISO, also take part in the work IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization Draft International Standards adopted by the technical committees are circulated to the member bodies for voting Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote International Standard IS0 301 was prepared by Technical Committee ISORC 28, Petroleum products and lubricants This second edition cancels and replaces the first edition (IS0 301 3:1 974), which has been technically revised, in particular with the inclusion of annex A Annex A forms an integral part of this International Standard IS0 997 All rights reserved Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher International Organization for Standardization Case postale 56 l CH-1 21 Geneve 20 l Switzerland Internet central isoch c=ch; a=lOOnet; p=iso; o=isocs; s=central x.400 Printed in Switzerland ii I NTERNATI ONAL STANDARD Petrol eu m produ cts of avi ati on fu el s WARNI NG wi th an d Th i s i ts Th e Th i s u se heal th u se of thi s I nternati onal I t i s the - I nternati onal Standard responsi bi l i ty practi ces an d Determi n ati on of the determi ne Standard does the I nternati onal Standard are present Normati ve u ser revi si on, regi sters speci fi es i n avi ati on stan dards Standard and possi bi l i ty a procedu re turbi ne fu el s i nvol ve to h azardou s address I nternati onal of regul atory for determi ni ng or avi ati on parti es of appl yi ng of cu rrentl y contai n At the to provi si ons ti me of agreemen ts the val i d most wh i ch, publ i cati on, based recent I nternati onal on al l of the Standard to l i mi tati ons materi al s, safety establ i sh pri or to operati ons probl ems an d associ ated appropri ate safety u se the temperatu re bel ow wh i ch sol i d hydrocarbon gasol i nes edi ti ons throu gh the thi s reference edi ti ons i nternati onal of the in i ndi cated standards thi s Standard l i sted text, were bel ow val i d are consti tu te Al l provi si ons stan dards encou raged Members to of I EC are of thi s su bj ect i nvesti gate and I S0 to the mai ntai n Stan dards 31 70: 988, Petrol eu m l i qu i ds - Man u al I S0 31 71 : 988, Petrol eu m l i qu i ds - Au tomati c sampl i ng pi pel i ne sampl i n g Defi n i ti on s For the pu rposes freezi ng temperatu re of thi s appl i cabi l i ty I S0 may purport poi nt referen ces fol l owi ng I nternati onal not of th e freezi ng Scope crystal s Th e - equ i pmen t I S0 301 3: 997(E) @ I S0 of thi s I nternati onal poi nt: Th e temperatu re of the test sampl e crystal l i zati on Standard poi nt: the fol l owi ng at wh i ch i s al l owed sol i d defi ni ti ons hydrocarbon appl y: crystal s, formed on cool i ng, di sappear wh en the to ri se Th e temperatu re at wh i ch crystal s of hydrocarbons fi rst appear wh en the test sampl e is cool ed Th e Pri n ci pl e sampl e contai ni ng tu be, contai ni ng a cool ant Du ri ng the test the cool i ng sampl e, a sti rrer, col l ar cycl e the test sampl e and i s sti rred thermometer, vi gorousl y is pl aced and exami n ed in a vacu u m fl ask for the formati on of Q ISC IS0 301 3:1 997(E) crystals When crystals are observed, the temperature is recorded as the crystallization point The jacketed sample tube is then removed from the coolant and the test sample allowed to warm up slowly Stirring continues until all crystals disappear, at which point the temperature is recorded as the freezing point Reagents and materials 5.1 Coolant Use one of the following liquids specified in 5.1 l to 5.1 in combination with solid carbon dioxide (5.1 5) or liquid nitrogen (5.1 6) under the specified conditions only Propan-2-01 [(CH&CHOH], 5.1 l NOTE - commercial grade of dry propanQ-ol Propan-P-01 is the preferred liquid for use as the coolant 5.1 Ethanol (C2H,0H), commercial grade of dry ethanol 5.1 Acetone (CHsCOCHs), commercial grade, provided it does not leave a residue 5.1 Methanol (CHsOH), commercial grade of dry methanol 5.1 Carbon dioxide (solid) or “dry ice”, commercial grade WARNING - Extremely cold, - 78 “C Liberated gases can cause suffocation NOTE - Mechanical refrigeration is permitted provided that the coolant temperature is in the range - 70 “C to - 80 “C 5.1 Nitrogen (liquid), commercial grade Use only when determining the freezing point of aviation gasolines, or if the freezing point of the aviation turbine fuel is lower than - 65 “C WARNING - Extremely cold, - 96 “C Liberated gases can cause suffocation 5.2 Nitrogen gas or dry air, a supply of nitrogen gas of low moisture content or dry air shall be used if moistureproof collar A is utilized 5.3 Fibreglass, 5.4 Dehydrating commercial grade, for use in moisture-proof collar B agent Use one of the following: 5.4.1 Calcium sulfate (CaS04), granulated anhydrous calcium sulfate, for use as a desiccant in moisture-proof collar B, or to assist in drying the nitrogen gas or air (5.2) used with collar A 5.4.2 Silica gel, mm, for use as a desiccant in moisture-proof collar B, or to assist in drying the nitrogen gas or air (5.2) used with collar A I S0 301 3: 997(E) Q I S0 Apparatu s See fi gure J acketed j acketed mou th of the sti rrer passes sampl e sampl e Col l ar, tube tube as tube, an d shal l shown a doubl e the outer be cl osed i s ei ther wal l ed, gl ass wi th unsi l vered j acket a cork fi gure or 3, bei ng stopper an d vessel , fi l l ed, si mi l ar to a Dewar at atmospheri c supporti ng the moi sture-proof to fl ask; pressure, thermometer i nhi bi t the the wi th and col l ar i ngress space between the or r The whi ch the dry ni trogen of through moi sture i nto the test sampl e Sti rrer, - NOTE a brass Vacu u m sampl e fl ask, an rod, , mm i n di ameter, bent i nto a smooth three l oop spi ral at the bottom, vacu u m vol u me fl ask of cool ant of (5 ) the and di mensi ons permi t the sh own in necessary fi gure depth Th e capaci ty of i mmersi on be conformi ng to annex A preparati on Gl assware Al l gl assware shal l be cl ean an d dry before use Col l ar Assembl e the col l ar Col l ar type (6 2) A, thermometer fl ush wi th (6 5) ni trogen and sti rrer (6 3) or dry r (5 2) i nto the cork before fi tti ng to the j acketed sampl e tube, an d the enti re determi nati on NOTE - Th e r can be effecti vel y dri ed by passi ng through absorbent tubes fi l l ed wi th dehydrati ng agents (54 2 Col l ar type B, fi l l wi th Th e fi bregl ass shal l than or wh en shal l of the j acketed tube Apparatu s unsi l vered to hol d an adequ ate Thermometer, steel sti rrer can be mechani cal l y actuated Th e suffi ci ent or stai nl ess months Vacu u m cool ant an d Obtai n sampl es a col our every chang e (5 3) fourth and a sui tabl e dehydrati ng test Th e dehydrati ng shows agent agent (5 shoul d or 2) be renewed as sh own at i nterval s and 2) i n fi gure of not more i t to be i neffecti ve fl ask I nsert suffi ci ent Sampl es fi bregl ass be repl aced throughout (5 ) to meet the i mmersi on depth requi rements sh own i n fi gure sampl i n g i n accordance wi th I S0 31 70, I S0 31 71 or an equi val ent nati onal standard I S0 301 3: 997( E) @ EC Di men si on s Sti rrer Moi stu re- proof , - - - Th ermometer col l ar -“1 Cork stopper J acketed outer sampl e tube: i nt : i nner tube: tube ext : ext : i nt : Un si l vered 30 m m 26 m m 22 m m mm vacu u m fl ask - 0i n t ?Ommmi n j /Cool ant - Sol i d Fi gure - Apparatu s for determi ni ng the freezi ng C arbon poi nt di oxi de of avi ati on fuel s i n mi l l i metres Q I S0 I S0 301 3: 997( E) Di men si on s i n mi l l i metres : B I nl et for -or I dry r ni trogen I / I nsert r Fi gure - i nto cork (sti rrer passes through tube) Moi sture- proof col l ar - Dehydrati ng type A agent - Fi breg l ass -Dehydrati ng I nsert -(sti rrer through Fi gure - Moi sture- proof agent i nto cork passes tube) col l ar type B I S0 3 : 9 7( E) Proced u re Tran sfer wi th th e mm Cl amp of d i oxi d e of th e wh e n on e Du ri n g of th e bottom sampl e sh al l maki n g per l oops sampl e of th e tu be be so cl ean col l ar; it exten d s m ake test sti r an d to d i oxi d e observati on s, an d d ry ad j u st j acketed th e sampl e th ermometer tu be ( ) posi ti on so Cl ose th at i ts th e tu be bu l b is ti g h t1 mm t tu be th at th e carbo n secon d th e an d approxi matel y th rou g h ou t n ot to th ermometer ad d sol i d cycl e at th e cool i n g cl ou d fi rst th e cycl e approxi matel y Ho we ve r Wh e n test wi th th e vacu u m mm bel ow cool an t fl ask th e l evel ( 4) l evel of i n th e tai n i n g th e th e cool an t vacu u m cool an t Ad d sol i d Th carbo fl ask n i trog en sampl e per th e 20 th e l i qu i d test , cycl e s tact to mai n tai n to th e i n to mm ti n u ou sl y, secon d Sti r bottom of th e th e movi n g test th e sampl e j acketed sti rrer from sampl e up top tu be to or an d d o wn bottom, travel at a taki n g above rat, car! th e tes su rface appears water of sti rrer, n ecessary Do n ot sti rrer sampl e’ s ml sampl e as - th e j acketed test ( 5) Exce pt th at + cen tre th e between th e th e th e WARN I N G ml h ol d i n g above su rface 25 cork sh ou l d exami n e “C su ch appeared formati on - an d a an d cl ou d th e n ot appear, a d escri pti on of crystal s test d oes i s n oted , of sampl e for i n crease n ote th e in th e presen ce i n ten si ty observati on as in of th e th e crystal s Di sreg ard temperatu re report, is an y l owered ; speci fyi n g th e cl ou d th i s is temperatu re th e due t wh e, i ts persi sten ce record th e temperatu re as th e observed crystal l i zati on poi n t N OTE S d i ffu sed , cool , A I f i t beco me s be m ay seen d i ffi cu l t removed temperatu re from of th e be to i s recommen d e d vi ew th e th e cool an t sampl e to d i sappear th en l i g h t sou rce an d by removi n g appearan ce for a tu be n ot sampl e sh ou l d th e sampl e i n vi ewi n g of crystal s peri od al l ow th e Th e sampl e observed to assi st th en to du e exceed i n g warm from th e g ase s s u n ti l be repl aced tu be to th e formati on rel eased I f crystal s i t i s “C wh e n th e an d by th e are warmer i n th e cool an t cool an t an d d i sappearan ce fou n d th an th e al l owed cool an t, th e to al read y h ave temperatu re to cool temperatu re of th e crystal s of th e Th e j acketed sampl e formed , wh e n th e th l crystal s an crystal l i zati on sampl e i s sl i g h tl y tu be n ote poi n t warmer ma th al th e n oted temperatu re Wh e n ti n u e warm th e up a th e observed observed 1 rate of Observe freezi n g Expressi o n Correct h as on e th e test sampl e been cycl e an d d etermi n ed , per secon d wh e n th e remove an d ,5 crystal s th e cycl es j acketed per compl etel y sampl e secon d , an d d i sappear, tu be from al l ow record th e th e th e test cool an t sampl e temperatu re tc a: poi n t of observed freezi n g poi n t between resu l ts freezi n g or temperatu re an d crystal l i zati on crystal l i zati on by l i n ear poi n t is correl ati on poi n ts between Report th e by two appl yi n g th e cal i brati on corrected rel evan t th ermometer temperatu res, freezi n g poi n t to th e correcti on obtai n th e n earest 0, Wh e n correcti on at th t th e “C Preci si o n preci si on of th i s meth od , Repeatabi l i ty, 1 l Th e d i fferen ce stan t wou l d between operati n g exceed r = 0, crystal l i zati on at sl owl y observed Th e th e sti rri n g “C th e as obtai n ed by stati sti cal exami n ati on of i n ter- l aboratory test resu l ts, i s as fol l ows: r su ccessi ve d i ti on s fol l owi n g on val u e test resu l ts, i d en ti cal i n on l y test on e obtai n ed materi al , case by in i n twen ty th e th e sam e n ormal operator an d wi th correct th e same operati on of apparatu s th e test unde meth od Q I S0 1 I S0 on R Reprodu ci bi l i ty, Th e di fference nomi nal l y fol l owi ng between i denti cal val u e 301 3: 997(E) two test si ngl e and materi al , i n onl y one case i ndependent i n the normal resu l ts, and obtai ned correct by di fferent operati on of the operators test i n di fferent meth od, wou l d l aboratori es exceed the i n twen ty R = 2, “C NOTES Th e preci si on h as been determi ned accordi ng to I S0 4259 except that the rou ndi ng rul es have not been appl i ed i n thi s i n stance 12 Th e sampl e matri x on wh i ch the preci si on of thi s standard i s based di d not i ncl ude avi ati on gasol i ne Test report Th e test report shal l contai n a) a reference b) al l detai l s c) the resu l ts d) an y devi ati on, e) the date of the test at l east the fol l owi ng to thi s I nternati onal n ecessary of the test Standard; for the compl ete (see cl au se by agreemen t i nformati on: i denti fi cati on the produ ct tested; 0) ; or otherwi se, from the procedu re speci fi ed; I S0 301 3: 997(E) An n ex A (normati ve) Th ermometer A Th e t h ermometer i n shal l descri bed Tabl e - A meet Requ i remen ts th e for of the freezi ng speci fi cati on requ i remen ts the g i ven thermometer poi nt i n tabl e for of avi ati on the “C to + 20 “C - I mmersi on Total 80 Gradu ati on s at each 0, Lon g er at each “C an d Fi g u red Scal e Expan si on Overal l St em “C “C “C at each error determi nati on fuel s Ran g e l i nes “C n ot to exceed ch amber permi tti n g h eati n g to 45 “C 0 m m + 5m m l en gth di ameter 6, m m to 8, m m Bu l b l en gth 8mmt o1 6mm Bu l b di ameter n o greater Bu l b s h ape cyl i ndri cal Len g t h of g rad u at ed Di stan ce from A porti on bott om of bu l b to “C l i ne 70 m m to 21 220 mm pl n Li qu i d col ou r perman en t Fi l l i ng above g as stem mm maxi mu m Top fi ni sh l i qui d t h an or ri n g u n d er red pressu re N OTES A Th ermomet er type I P 4CI ASTM 1 4C meets the above A Tol u en e A The th ermometer i s sui tabl e as the actuati ng l i qui d shal l have a val i d cal i brati on certi fi cate requ i rements I S0 I CS 301 3: 997( E) 75 60 20 Descri ptors: Petrol eu m poi nt Pri ce based on pages Produ cts, au tomoti ve fu el s, avi ati on fu el s, tests, ph ysi cal tests, l ow temperatu re tests, determi nati on, sol i di fi cati c