Tiêu chuẩn iso 03400 1997 scan

I S0 I N TE RN ATI ON AL 400 STAN D ARD Th i rd e d i ti o n 997- 04- C i g arettes sm o ke - D eterm i n ati o n co n d en sate s - of al kal o i d s in S pectro m e tri c m eth o d C i g arettes M kth od e - D G term i n ati o n d es al cal o i ’ d es d an s /es co n d en sats de fu m 6e - spectro m ktri q u e R e fe re n ce I S0 n u m be r 40 : 9 ( E ) I S0 40 : 9 7( E ) Fo re wo rd I S0 (th e I n tern ati on al worl d wi d e bod i es) Th e carri ed ou t wo rk i n terested in a establ i sh ed wi th D raft al so I n tern ati on al to m em ber I n tern ati o n al g o vern m en tal th i rd B 26, an d wo rk th at been co m m i ttee n o n -g overn m en tal , I S0 col l abo rates C om m i ssi on by th e fo r in cl osel y (I E C ) tech n i cal vo ti n g approval on com m i ttees P u bl i cati on by I S0 400 was To bacco an d to bacco can cel s h as of on bod y h as al l at l east 75 are as % of an th e a vo te wh i ch an d th e bod i es req u i res ed i ti on A in ad opted m em ber S tan d ard 400 : 89 ) , represen ted n orm al l y stan d ard i zati on casti n g l SO/TC is m em ber com m i ttee a m em ber E ach tech n i cal E l ectrotech n i cal Stan d ard Co m m i ttee a is (I S S tan d ard s co m m i ttees be part Stan d ard s th e bod i es An n exes to take bo d i es I n tern ati on al wh i ch ri g h t I n tern ati o n al I n tern ati o n al (I S0 fo r Stan d ard i zati on ) stan d ard s tech n i cal el ectrotech n i cal ci rcu l ated Th i s prepari n g I S0 th e I SO, th e of n ati on al o rg an i zati on s, wi th m atters of su bj ect h as I n tern ati o n al l i so n of th ro u g h for Org an i zati o n fed erati on th i s an d been prepared repl aces tech n i cal l y I n tern ati o n al by Tech n i cal pro d u cts th e secon d ed i ti o n revi sed are Stan d ard fo r i n fo rm ati on o n l y Al l I S0 997 ri g h ts re se rve d reprod u ced i n cl u d i n g or U n l e ss u ti l i ze d in ph otocopyi n g oth erwi se an y an d fo rm spe ci fi e d , or by m i cro fi l m , an y no wi th ou t pu bl i sh er I n tern ati on al Org an i zati o n Case 56 postal e I n tern et x 400 P ri n ted ii CH -1 21 for Stan d ard i zati on G en eve 20 l Swi tzerl an d ce n tral @ i so ch c= ch ; in l a=400n et; S wi tze rl an d p= i so ; o = i so cs; part m e an s, s= cen traI of th i s pu bl i cati o n e l e ctro n i c pe rm i ssi o n in or wri ti n g m ay be m e ch an i cal , fro m th e I N TE RN ATI ON AL STAN D ARD C i g arettes D eterm i n ati o n - co n d e n sates of S pectro m e tri c al kal o i d s 40 : 9 7( E ) in sm o ke m eth o d S cope Th i s I n tern ati on al ci g arette sm oke n o rm al l y carri ed d eterm i n ati o n Stan d ard ou t sm oke to u se Th i s an becau se by of Th e val i d of Stan d ard u se m ad e th e 43 87 I S0 d eterm i n es th e 03 5) al kal o i d s th e expressi on to tal th i s by is th e of al so al kal o i d s sm oke appl i cabl e are of th i s in are to th e sm o ki n g d eterm i n ati on th at d eterm i n ati o n in of m n stream n o n -stan d ard co u n tri es d escri bed n ot in n i co ti n e of n i co ti n e a po si ti on in I n tern ati on al sm o ke Stan d ard resu l ts al kal oi d s, th an of m eth od for In wh ereas separati o n oth er d eterm i n ati o n col l ecti o n obtai n ed m eth o d g as-ch rom atog raph i c of H owever, m eth od , th e an d g as-ch rom atog raph y al so by in spectrom etri c d en sates of (see perform ed n o te am o u n ts th i s are tai n I n tern ati on al stan d ard s stan d ard s be stan d ard s of Al l th e th e ci g arettes n i co ti n e I S0 03 Occasi o n al l y, in som e types d eterm i n es d i fferen ces of can on l y o ccu r to bacco referen ces fol l o wi n g pro vi si on s I S0 sm oke sol u ti o n s Stan d ard vi rtu e N o rm ati ve wi th fo r of g as-ch ro m atog raph i c appropri ate m i n or a m eth o d sm o ki n g ci g arette speci fi es sh o u l d I n tern ati o n al n i coti n e in 43 87 th e Th e acco rd an ce d en sate co n d en sate an d in n i coti n e I S0 in speci fi es co n d en sates of N OTE I S0 @ I S0 are su bj ect en cou rag ed l i sted bel ow to pro vi si on s Stan d ard to revi si on , i n vesti g ate M em bers of wh i ch , At th e an d th e th ro u g h ti m e parti es po ssi bi l i ty I E C an d of I S0 referen ce pu bl i cati o n , to of ag reem en ts appl yi n g m n tai n th i s of text, ed i ti o n s based th e reg i sters in th e m ost on th i s recen t cu rren tl y sti tu te i n d i cated were I n tern ati o n al ed i ti o n s val i d of th e I n tern ati o n al Stan d ard s I S0 696: 87, Water I S0 43 87: 99 , C i g arettes a rou ti n e I S0 76: 97, m eth od an al yti cal u si n g an al yti cal - D eterm i n ati on sm o ki n g Tobacco u se of - to tal Speci fi cati on an d an d n i co ti n e-free test d ry m eth od s parti cu l ate m atter u si n g m ach i n e an d tu n g sto si l i ci c l aboratory to bacco pro d u cts - D eterm i n ati on of n i co ti n e pu ri ty - G ravi m etri c aci d P ri n ci pl e D i sso l u ti o n of for an an d al i q u o t rem oval of th e sm oke po rti on of of n eu tral d en sate th e an d sol u ti o n aci d from in two th e m n stream steps steam - vo l ati l e sm oke Aci d i fi cati o n su bstan ces by of in th e a so l ven t so l u ti on d i sti l l ati on Steam wi th fol l owed a by d i sti l l ati on m i n eral m aki n g aci d th e I S0 sam e th e sol u ti o n stron g l y absorban ce expressed @ I S0 3400: 997(E ) as of th e al kal i n e an d d i sti l l ate d i sti l l ati o n from th e al kal o i d s S pectrom etri c an d cal cu l ati on m easu rem en t of th e g rad e in %, m ay al so to al kal o i d of ten t Reag en ts U se on l y reag en ts of recog n i zed an al yti cal 69 P ro pan -2 -01 Sod i u m h yd roxi d e Su l fu ri c aci d sol u ti o n , c(H , SO, ) = 4 Su l fu ri c aci d sol u ti o n , c(H , SO, ) = , 02 5 N i co ti n e, S to re Test at th e [(CH , ) , OCto +4 n i co ti n e sol u ti o n , pu ri ty OC an d pu ri ty extracti on 98 of accord an ce wi th = m o l /l m o l /l m ol /l l i g h t acco rd an ce N i co ti n e water % excl u d e in an d sol ven t c(N aOH ) g rad e wi th h yd rog en I S0 76 tartrate, minimum pu ri ty 98 be u sed Apparatu s U su al It CH OH ] , minimum N OTE l abo rato ry Steam is an to n i co ti n e th e (6 ) N OTE cyl i n d ri cal , sh al l th at i tem s si sti n g th e of of of extracti on th e Th e th e th e n i co ti n e at is a parts steam so l ven t reco very at d i ag ram s exam pl es l evel in d i sti l l ati o n (4 ) better l i sted of th an su ch apparatu s th at a ml approxi m atel y 98 % If n ot, reg u l arl y al i q u o t mg o pti m i ze P repare po rti o n U se by a co n tai n s th i s as a m o d i fi cati o n test of of Oth er apparatu s apparatu s cu rren tl y m ay al so u sed be (an n ex u sed A, provi d ed fi g u res th at th e A to resu l ts A ) are obtai n ed sam e ch am ber verti cal l y i n l et be fo l l owi n g perfo rm an ce am ou n t en su re as th e D i sti l l ati o n a steam th e rate g i ven I th e u si n g kn own d i sti l l ati o n are ch eck an d an d apparatu s, sol u ti on accu ratel y porti o n apparatu s d i sti l l ati o n essen ti al pu re It th e d i sti l l ati o n n i coti n e I S0 A of al kal i n e i ts po ssi bl e m ou n ted d i sti l l ati o n ch am ber of abo u t 50 ml to 00 ml capaci ty, wh i ch h as d u ri n g th e base to h eat th e ch am ber in ord er sph eri cal j oi n t to m n tai n a co n stan t li qu id l evel d i sti l l ati o n D i sti l l ati o n J acketed P l u g -type spl ash coi l h ead d en ser, fu n n el , or oth er wi th system for ad d i ti o n fi tti n g of on to sod i u m th e d i sti l l ati on h yd roxi d e spl ash so l u ti on h ead (5 2) I S0 @ I S0 It is i m portan t escape th at th ro u g h Spectrom eter, M atch ed Larg er d u ri n g th e tap q u artz m atch ed Vo l u m etri c fl asks, 5 On e-m ark pi pettes, G l ass Fi l ter fu n n el s, paper, h avi n g cel l s of of of a wavel en g th cel l s, q u artz i n tro d u cti on th e sod i u m h yd roxi d e sol u ti on nm nm (4 2) steam d oes n ot stopper co veri n g th e or 40 : 9 7( E ) an m ay be capaci ty of o pti cal u sed 250 capaci ti es d i am eter fast-fi l teri n g for ml, 55 of fro m path 23 l en g th very wi th ml, abou t g rad e, ran g e l ow of an d 29 g l ass 25 (See al so N o te 7) cm co n cen trati on s g ro u n d ml to of n i co ti n e sto ppers ml mm a d i am eter to su i t th e g l ass fu n n el (5 6) P ro ced u re P reparati o n P repare th e kn own d i sc, u se 50 stan d ard Test ml sam pl e of th e d i ssol vi n g For so l ven t th e sm o ki n g as th e test mg 44 An al ysi s sam pl e an d th e th e at of d en sate d i sc, sh ou l d OCto d i sso l vi n g sm oke mm +4 be u se obtai n ed ml of perform ed OC an d sm o ke 25 as excl u d e th e by m ach i n e-sm oki n g so l ven t so on as (4 ) ; possi bl e fo r th e bu t if a 92 mm sto rag e is l i g h t d en sate, refer to I S0 43 87 porti o n , to mg an of al i q u ot porti on (V, ) of th e sm oke d en sate sol u ti o n co rrespo n d i n g al kal o i d Th i s speci fi cati o n Take care d u ri n g can n ot be m et fo r l ow n i coti n e ci g arettes D i sti l l ati on WARN I N G - appro pri ate safety N OTE th at Th e I n trod u ce th e th e ml of d i sti l l ate in d i sti l l ate su l fu ri c ml th rou g h a of so l u ti on th e so d i u m C ol l ect l i ttl e water wh i l e 20 speci fi ed oth er (6 2) aci d beaker th e If d el i very (4 ) are i n to sod i u m h yd roxi d e is bei n g ad d ed an d wear tu be E n su re th at to Term i n ate 230 th e of an d th ese rel ate q u an ti ti es ch am ber start th e 250 ml th e en d of (4 2) , d i sti l l ate d i sti l l ati on th e of to th e m ay type be an d tu be cl o si n g ri n se is th e Rem ove d i sti l l ati o n C ol l ect rem ove vol u m etri c th e th e d i sti l l ati on d i sti l l ati on , a sol u ti on ml su bcl au se u sed , d i sti l l ati on (4 ) i n to th i s is of apparatu s m od i fi ed provi d ed sam e stoppi n g h yd roxi d e ml th e th e sol u ti on Wi th o u t in apparatu s o btai n ed porti on su l fu ri c I n set- t d i sti l l ati on q u an ti ti es resu l ts test a aci d in th e th e eq u i pm en t speci fi ed wi th by ci g arettes sto re N OTE sam pl e porti on abo u t test of th en For to test n u m ber i n evi tabl e Take, of th e th e fl ask th e i n l et fl ask sti l l beaker (5 4) i m m ersed in fu n n el wh i l st E n su ri n g apparatu s abou t an d as aci d th e ri n si n g th at ml S l o wl y l ast th e th e ml Ad d of d i scard tai n i n g th e (5 ) 00 th e ad d d ro ps is th e of d el i very fl ask th e at pass tu be roo m I S0 @I S0 40 : 9 7( E ) tem peratu re, d i l u te spectro m etri cal l y to th e N OTE before th e m ark al kal oi d s I f fi l trati on u se, th e (vol u m e in is fi l ter th e l /J sm oke n ecessary, paper wi th water Mix d en sate ei th er sh o u l d be th e fi rst wash ed an d Fi l ter 50 wi th u se i f th e ml th i s so l u ti on so l u ti on of fi l trate a su ffi ci en t is sh ou l d am ou n t to n ot d eterm i n e cl ear be of d i scard ed water an d o r, th en d ri ed D eterm i n ati o n U si n g 59 to th e nm 250 I f th e 82 wi th nm (VJ abo ve Th e vol u m e wi th (5 2) , th e d i sti l l ate m easu re ag n st a at 259 exceed s th e as th e nm su l fu ri c referen ce (V’ ) in th e referen ce absorban ce so l u ti on of of ml th e of fi l trate th e at su l fu ri c wavel en g th s aci d of so l u ti on 23 (4 ) nm, d i l u ted water absorban ce vol u m e al kal o i d s spectrom eter an d ml of aci d so l u ti on al i q u o t is , 8, d i l u te so l u ti o n al so porti o n d i l u ted (VJ an (4 4) wi th I f th e al i q u ot an d porti o n m easu re su l fu ri c abso rban ce th e aci d at (I / ‘ ) o f so l u ti on 259 th e d i sti l l ate absorban ce nm is (4 4) l ess of to th an th e 0, to th i s a su i tabl e so l u ti o n sam e u se as su i tabl e l arg er cel l s (5 ) C arry ou t two Cal cu l ati on Th e al kal o i d ci g arette, H of an d of expressi o n ten t fo r nit d eterm i n ati on s each H n i c of sm oki n g th e test sam pl e u n d er i d en ti cal co n d i ti on s resu l ts th e ru n sam e sm o ke is g i ven d en sate, by th e expressed as n i co ti n e in m i l l i g ram s per fo rm u l a wV, V, (1 ) - a/VJ p wh ere a is th e abso rpti vi ty sol u ti on A is th e (4 4) (i (d ecad i c e corrected wavel en g th s of 4, i s th e o pti cal V, i s th e vo l u m e y i s th e al i q u o t V2 i s th e vo l u m e path of nm, 59 co effi ci en t) abso rpti o n m axi m u m (exti n cti o n ) nm an d 282 of of cal cu l ated n i coti n e 259 nm) from in g i ven th e , 02 in m o l /l of propan - 2-0 of d i sti l l ate I /, su l fu ri c aci d m l Sm g %m -‘ ; absorban ces m easu red at nm: + A282 l en g th porti o n of at th e abso rban ce 23 A23 I exti n cti on (2) th e cel l , in sol u ti on u sed from for th e cen ti m etres; of th e cru d e sm oke d i sti l l ati on , al kal i n e in d i sti l l ati o n , co n d en sate, m i l l i l i tres; in m i l l i l i tres; in m i l l i l i tres; I S0 3400: 997(E) An n e x A (i n fo rm ati ve) D i ag ram s of apparatu s cu rren tl y u se d D i m en si on s 50 - Stoppe r - A h II _Q, ext - i 60 A Q>ext 54 @ ext 32 @ ext Th orpe Fron t vi e w N OTE S Al l g l ass S to pco cks: is m ed i u m mm wal l bore borosi l i cate P TFE Fi g u re A - E xam pl e of apparatu s cu rren tl y in u se d en ser in m i l l i m etres I S0 3400: 997(E) @ I S0 D i m en si on s E l e ctri cal Fi g u re in m i l l i m etres t A - E xam pl e of apparatu s cu rren tl y in u se I S0 @ I S0 3400: 997(E) D i m en si on s Ad apter l i quid for in m i l l i m etres th e sam pl e R S 29 e xt - 30 P TFE bore 35 @ ext R CN 29 65 ’ CN @ ext E r c X : Ste am _- -L Stan d ard d en seran d N OTE - Al l g l ass is @ ext Q, e xt 85 m ed i u m wal l Fi g u re d i sti tl ate borosi l i cate A - E xam pl e of apparatu s cu rren tl y in u se re ce i ve r I S0 @ I S0 An n ex 40 : 9 7( E ) B (i n fo rm ati ve) B i bl i o g raph y [I ] I S0 03 5: 91 , ch rom ato g raph i c [Z] Wi l l ets 950, [3 ] pp C Ci g arettes - D eterm i n ati on of n i co ti n e in sm o ke d en sates - G as- m eth o d O , S wai n M L , Co n n el l y J A , Bri ce B A An al yti cal C h em i stry, 22 , N o 3, M arch 43 -43 l SO/l E C l abo ratori es Guide 25: 90 , G en era/ req u i rem en ts fo r th e com peten ce of cal i brati on an d testi n g I S0 @ I S0 40 : 9 7( E ) I CS 65 60 D e scri pto rs: P ri ce based tobacco, on pag es ci g arettes, sm o ke , ch e m i cal an al ysi s , d ete rm i n ati on of ten t, al kal o i d s, spe ctro m e tri c m eth od