Tiêu chuẩn iso 11437 1 1994 scan

I S0 I N TE RN ATI ON AL S TAN D AR D 1 43 7- I Fi rst ed i ti on 9 4- l N i ckel al l oys trace- el emen t atomi c by of el ectroth ermal spectrometri c - : Ge n eral Al l i ag es de spectrom&ri e Par- ti e ten t absorpti on me t h o d Part Determi n ati on - 2- 01 7: req u i remen t s n i ckel - Dos ag e d ’ absorpti on Caract&i sti q u es d es an d 61 6men ts- traces atomi q u e g &Wal es s ampl e Ei exci tati on et mi se en - d i ssol u ti on M &h o d e par Bl ectroth ermi q u e sol u ti on de ’ 6ch an ti l l on Re f e ren ce I S0 - 1 43 7- l n u mb e r :I 9 4( E) I S0 1 43 7- : 9 4( E) Fo rewo rd I S0 ( th e I n tern ati on al fed erati on of of prepari n g tech n i cal wh i ch stan d ard s I n tern ati on al co mmi ttees a tech n i cal represen ted an d Org an i zati on n ati on al on Each ( I EC) on Draft cl osel y al l matters of I n tern ati on al ci rcu l ated to Stan d ard in th e req u i res been wi th I SO, by at ou t i n terested in h as take worl d wi d e part Th e wo rk th rou g h a I S0 su bj ect th e org an i zati on s, al so a ri g h t for to be g overn men tal in th e El ectrotech n i cal wo rk I S0 Co mmi ssi o n stan d ard i zati on ad opted for is bod i es) carri ed establ i sh ed I n tern ati on al bod i es approval n ormal l y bo d y el ectrotech n i cal me mbe r member I n tern ati on al Stan d ard s th e is h as l i son wi th Stan d ard i zati on ) ( I S0 me mber co mmi ttee n on - g overn men tal , col l aborates Stan d ard s co mmi ttee th at for bod i es by th e voti n g l east 75 tech n i cal Pu bl i cati on % of th e co mmi ttee s as me mber an are I n tern ati on al bod i es casti n g a vote I n tern ati on al l SO/TC n i ckel I S0 Stan d ard 55, 1 43 - 1 43 7- n i ckel co n si sts of th e Determi n ati on absorpti on was of by Tech n i cal Su bco mmi ttee spectrometri c SC 4, Co mmi ttee An al ysi s of 2: Determi n ati on of l ead - Part 3: Determi n ati on of bi smu th - Part 4: Determi n ati on of si l ver fo rms i n formati on an u n d er co n ten t th e by g en eral ti tl e el ectroth ermal Ni ckel ato mi c meth o d : Part I S0 Gen eral parts, - A 7: fol l owi n g trace- el emen t Part req u i remen ts i n teg ral part of an d sampl e d i ssol u ti on ten t co n ten t ten t th i s part of I S0 1 43 An n ex B is for on l y 994 Al l ri g h ts or u ti l i zed reserved m i cro fi l m , in an y in Postal e U n l e ss fo rm wi th ou t I n tern ati on al Case Pri n ted prepared al l oys, - An n e x ii I S0 an d al l oys al l oys Ni ckel or oth erwi se by an y pe rmi ssi o n Org an i zati on 56 Swi tze rl an d l in wri ti n g for CH- 21 speci fi ed , me an s, no el ectron i c from th e part or of pu bl i sh er Stan d ard i zati on Ge n e ve 20 l th i s pu bl i cati on mech an i cal , Swi tze rl an d i n cl u d i n g may be reprod u ced ph otocopyi n g an d I S0 I S0 1 43 7- : 9 4( E) I n trod u cti on Th i s part wh i ch in of n i ckel St an d ard s, the it 1 43 met h od s al l oys Al t h ou g h test I S0 speci fy by to be th e el ectrot h ermal an al yti cal is is for possi bl e met h od s to u s ed in j u n cti on d etermi n at i on at omi c are d et ermi n e of absorpt i on speci fi ed mo re in t h an wi th i n di vi du al th e ot h er trace parts el emen t s spect romet ry i n d epen d en t on e el emen t I n tern ati on al on a si n g l e sol u ti on I ll ‘, I N TERN ATI ON AL N i ckel S TAN D ARD al l oys co n t en t by el ect ro t h ermal meth od of t race- el emen t at o mi c abs o rpt i o n - re q u i re me n t s an d s am p l e d i ssol u t i on I S0 Sco p e 385- l Part I S0 1 I S0 sorpti on 1 43 speci fi es met h o d s emen t s in g i ven cl au se in 1 43 l oys are of be Typi cal g i ven Th i s in part q u i remen t s sampl e, test an d in u s ed parts ad d e d in of I S0 1 43 th e of trace of s o me by speci fi es of an d Ot h er parts of n i ckel al - g en eral of i n d i vi d u al an d th e ab- fol l owi n g 648: 977, th e pro- st an d ard s in tai n th i s text, provi si on s sti tu te I S0 42: 983 , vol u met ri c th i s part of I S0 1 43 At the ti me I S0 ed i ti on s of st an d ard test to i n d i cated on part th i s g ate th e ti on s of I EC an d revi si on , of I S0 possi bi l i ty th e we re val i d parti es 1 43 of st an d ard s I S0 I n tern ati on al an d mai n t n St an d ard s are to Al l of i n d i cated reg i sters bel ow of g l assware - On e- mark Preci si on of repeatabi l i ty met h o d test an d by me t h o d s - Deter- reprod u ci bi l i ty i n ter- l aboratory for a tests Di ssol u ti on aci d an d of a test porti on h yd rofl u ori c in a mi xt u re of d i l u te n i tri c aci d Di l u ti on of th e tran sfer of an Ad d i ti on of ary, i n j ecti on an d i n to a test an sol u ti on al i q u ot to mod i fi er of a to an d /or a a pl asti cs smal l el ectroth ermal kn o wn vo l u me an d vi al d i l u en t, wh ere vo l u me of th e n ecesstest sol - reso n an ce l i ne atomi zer wh i ch , st an d ard s mo s t On e- mark of th e absorpt i on of th e from th e spect ru m of th e el emen t bei n g d e- pu bl i cati on , ag reemen t s th e - provi si on s en co u rag ed appl yi n g - Pri n ci pl e to co mpari s o n wi th th at of cal i brati on sol - tai n i n g th e s am e el emen t bas ed i n vesti - recen t ed i - M e mbe r s cu rren tl y an d are u ti on s su bj ect g l assware Laborat ory 5725: 986, termi n ed th e Bu ret tes fl asks mi n at i on en erg y of - speci fi ed 1 43 referen ces referen ce g l assware Laborat ory Me as u reme n t th ro u g h Laborat ory req u i remen ts pi pettes u ti on Th e 984, of repeatabi l i ty me t h o d s :I Gen eral re- ato mi c d i ssol u ti on cal cu l ati on eval u ati on th e th e el ectroth ermal : el - ran g es 1 43 s u bs eq u en t preparati on I S0 N o rmat i ve of ab- B me t h o d for reprod u ci bi l i ty oth er parts I S0 th e of cen trat i on oth er an al ysi s spectrometry, ced u res th e composi t i on s sorpti on at omi c d etermi n ati on in an n ex of for el ectroth ermal the al l oys, may I S0 for n i ckel el emen t s 1 43 7- : 94( E) : G e n e ral I S0 I S0 Det ermi n at i o n - spect romet ri c Part of Re ag e n t s val i d Du ri n g th e an al ysi s, u n l ess oth erwi se stated , u se on l y I S0 1 43 7- : 9 4( E) reag en ts ti l l ed of recog n i zed water or water an al yti cal of g rad e eq u i val en t an d on l y d i s- Th e d i sch arg e by Hi g h pu ri ty speci fi ed in metal s, th e 99, rel evan t part % of ( m/m) I S0 mi n i mu m, th e l amps aci d , pZO= I , 41 g /ml , Hyd rofl u ori c aci d , pzO = d i l u ted I,1 WARN I N G tati n g an d bran es, Hyd rofl u ori c corrosi ve ski n severe to h eal In th e is extremel y an d ski n case wel l wi th water an d wi th Aci d Carefu l l y an d 50 water mi xtu re ad d ml Mi x for ml th e h yd rofl u ori c an d of store in n i tri c a med i cal of vi al s, of capaci ty ml aci d ( p2, , = aci d ( 3) vol u metri c fl asks, of capaci ti es 50 ml vol u metri c an d 000 fl asks, ml , in of capaci ti es acco rd an ce wi th 00 I S0 ml , 042, ad vi ce I , 41 to g /ml ) 50 ml A Bu rettes, i si on s of of ml ) , 0, l of 0, 02 in capaci ti es ml ) an d 25 acco rd an ce IO ml ml ( g rad u ated ( g rad u ated wi th I S0 in 385- , in d i v- d i vi si on s Cl ass A of bottl e beakers, ml G l ass ml pl asti cs ( PTFE) are d i ssol u ti on 50 of reco mmen d ed ski n , Cl ass 4 u si n g me m - wh i ch co n tact se ek cu rren ts of el ectrod el ess ml Pl asti cs 00 50 wash 00 Pl asti cs an d i rri - mu co u s bu rn s of or +I 5 sl o w capabl e g /ml aci d to prod u ci n g at Pol ytetrafl u oroeth yl en e - operated be l amps as sh ou l d cath o d e man u factu rer capaci ty Ni tri c h o l l ow 1 43 spectrometer si n g l e- el emen t pu ri ty I S0 Pi pettes, in acco rd an ce wi th I S0 648, Cl ass A Mod i fi ers Prepare separatel y appropri ate part for of each I S0 metal as speci fi ed in th e to Mech an i cal 00 to Stan d ard of capaci ti es IO ~1 2, ~1 1 43 mi cropi pettes, 1 referen ce sol u ti on s, 00 mg /l of Vari abl e I O, mech an i cal ~ , fi tted wi th pi pette, pl asti cs of capaci ty posi ti ve d i spl acemen t ti ps metal Prepare separatel y rel evan t part of for I S0 each metal as speci fi ed in th e Sampl i n g Sampl i n g sampl e or, n ati on al l aboratory apparatu s, be preparati on carri ed ou t of by th e n ormal l aboratory ag reed Ato mi c absorpti on spectrometer of th i s Th e meth o d atomi zer g i ven atomi c in an d an n ex Th e backg rou n d capabl e of g raph i te fi tted meet Th e wi th th e an u sed corrector measu ri n g as a peak atomi zer tu be an d speci fi ed d i spu te, by th e pro- rel evan t I n ter- be rapi d h ei g h ts sh al l L’ vo v in cri teri a eq u i pped wi th record i n g an d be pl atform, th e l aboratory sampl e mi l l i n g s preparati on or of n ormal l y d ri l l i n g s th e an d sampl e is is no in th e fu rth er form mech - n ecessary el ectroth ermal performan ce sh al l an d of in Th e wash i n g spectro meter tu be spectro meter A g raph i te 1 43 be sh al l el ectroth ermal pyrol yti c absorpti on sh al l case Stan d ard tu rn i n g s, an i cal in an d preparati on Apparatu s Ord i n ary I S0 sam pl e an d sh al l ced u res Th e an d 1 43 fi tted or rel evan t areas wi th a a n ormal part pu re sampl e aceton e sh al l an d be d ryi n g cl ean ed in by r a syste m peak l aboratory wi th of of If th e cl ean ed u tes wi th brazed al l oy l aboratory by Th e pi ckl i n g sampl e d i sti l l ed aceton e, an d in sh al l water r tool s sampl e, are u sed th e sampl e d i l u te th en fol l owed d ri ed n i tri c in aci d th e sh al l for preparati on be a fu rth er few be wash ed several by several wash i n g s mi n ti mes wi th I S0 I S0 7 Pro ced u re 50 At omi ze ~ ) for th e the bl an k 1 43 7- : 9 4( E) presel ect ed sol u ti on vol u me Record th ree (I O ~1 to absorban ce measu remen t s Preparat i on of test sol u ti on - Ge n er al Ch eck met h od presel ect ed h i g h est Wei g h , to the n earest 0, 001 g, 0, 500 g of l aboratory s ampl e ( 2) sol u ti on (4 4) mai n t n an d Ad d th e 20 tran sfer ml Appl y of to the su ffi ci en t reacti on u nti l th e aci d 00 ml mi xt u re h eat to d i ssol u ti on cal i brati on for each Cool the rel evan t N OTE ni tri c sol u ti on part of an d I S0 50 compl et e porti on s of th e correspon d i n g aci d d i ssol vi n g bl an k test as d i rected in 1 437 I t may be di ffi cu l t aci d - h yd rofl u ori c proceed to d i ssol ve for t wo Bl an k al l may be cases, th e ad j u sted , pro- ou t n ati on , a s ame test th e q u an ti ti es of in paral l el s ame al l Preparat i on bu t a as the of d i rected wi th the proced u re an d d etermi u si n g the Cal i brat i on mean At omi c of Th e cal i brat i on in the an d g raph i t e h ei g h t peak an al ysi s I S0 t u be or are 1 43 stru cted an d area in an n ex part of I S0 1 437 th e for each el emen t , meas u remen t in to th e n ew the mo d e be ( peak u sed rel evan t g raph i te type in the part t u bes be bet ween of the o pt i mu m accord an ce vol u me IO th e at omi ze cord fu rn ace wi th i n j ected PI an d Starti n g th ree cal i brati on th e in of the th ree to absorban ce me an g raph s absorban ce cal i brati on val u es a val u es val u e ob- from th e sol u ti on obtai n ed g raph for th e rel ati n g obt n ed to per U si n g bl an k test th ei r remai n i n g for the an al yt e th e me an cal i brati on sol - cen trati on s (i n l i tre) of th e resu l t s mean sol u ti on cen t rat i on of absorban ce ( 51 , th e bl an k brati on cu rve ( 2) I f th e cal i brati on i n- th e obt n ed d et ermi n e test sol u ti on for th e from the an al yt e the cal i - s h o ws 50 i n to g i ven wi th the fu rn ace ~ , d epen d i n g absorban ce sol u ti on s th e vol u me on cal i brati on (I O measu remen t s PI ad j u st U si n g ch eck the measu remen t th e cal i brati on cal i brati on cu rve obt n ed cu rve h as dri fted accord i n g l y the th e to for th e me an d et ermi n e test absorban ce th e an al yte val u es obt n ed cen trati on of in t wo sol u ti on s sh al l sen si - presel ected th at t emperat u re i n stru cti on s an al yte th e an d Cal cu l at i on test measu red cal i brati on pg /l Expres s i on of ti vi ty in are mean s of ( ) 7, Th e 1to th ree of as A (I O Record man u factu rer Est abl i sh in the Con stru ct si g n i fi can tl y, pro g ramme vol u me sol u ti on s mi crog rams in measu re- measu remen t s i n teg rati on ) speci fi ed the an d d et ermi n at i on l i n es Con d i t i on by th ree sol u ti on s i n stru cti on s obt n ed th e absorban ce sol u t i on s rel evan t absorpt i on spectral test sol u ti on s absorban ce th e zero reag en ts the test Su bt ract for cal i brati on presel ect ed th e Preparat i on u ti on s Proceed the sol u ti on s the Cal cu l at e 2 the meas u remen t s bl an k Record at omi zi n g i s n ecessary test fol l owi n g by ~ ) of meas u remen t s of tai n ed Carry the of Repeat 7 50 certai n al l oys i n t h e I n su ch mi xt u re sl ope to sol u ti on s of At omi ze ~1 ) u n ti l mi xtu re ~1 di san d absorban ce th e (I O PTFE for i n i ti ate is cal i brati on the men t s beaker th e vol u me Repeat u n ti l th e th e sol u ti on s i n stru cti on s an al yte are g i ven cen t rati on s of in the an d remai n i n g obtai n ed sol u ti on s, 50 each ~ ) Reof the Su btract test th e sol u ti on test the ( sol u ti on s I) an al yte from fou n d cen trati on the in an al yte an d of th e bl an k cen t rat i on of I S0 1 437- : 994( E) Cal cu l ate sampl e, in th e g rams an al yt e per t on n e, t en t u si n g w th e of the test 2 of formu l a is PDF 20 to x m Th e resu l ts too is l arg e pri n ci pl e an in d et ermi n e from th e appl i ed if rel ati on if the oth er at of ou tl i er th e th e to % test i s th at wi th i n - l aboratory th e me an oth ers from l aboratory 95 Coch ran the a Di xon ’ s Bot h a set vari an ce l aboratory mean s fi d en ce I S0 tests is too tests is far were l evel wh ere i s the P per in an al yte l i tre, in cen trati on , the test in sol u ti on , mi crog rams as cal cu l ated 2 l ated Repeatabi l i ty accord i n g l evel 5; Resu l ts to of th e wi th i n - l aboratory F i s a di l u ti on of is m h ave the met h od s been in Stati sti cal Resu l t s g ramme were g i ven i n th e rel evan t part were Di xon th e in g rams, su bseq u en t of the test parts i n terl aboratory of of are I S0 at stati sti cal an d g i ven reprod u ci bi l i ty 5725 th e were 95 % an al ysi s, i n cl u d i n g bet ween - l aborat ory for each el emen t cal cu - fi d en ce in the st an d ard th e rel evan t 1 437 porti on I S0 1 43 Test Th e test report report a) a referen ce b) the resu l ts c) the n u mber d) an y e) an y sh al l to of i n cl u d e th e the th e met h o d fol l owi n g i n formati on : u sed ; an al ysi s; testi n g of i n d epen d en t repl i cati on s; an al ysi s from the eval u at ed tested tests to d evi ati on s part tests su bj ect ed 2 an d mass, Laborat ory 2 d at a factor 1 437; Preci si on Th e I S0 an d I S0 for accord i n g stati sti cal g i ven in i n terl aboratory I S0 to ou tl i ers 5725 I S0 by test pro- 5725 Th e the Coch ran I S0 u n u su al featu res operat i on 1 43 or n ot ed n ot reg ard ed d u ri n g i n cl u d ed as in opti on al th e an al ysi s; th i s part of I S0 An n e x 1 437- : 994( E) A ( n ormati ve) an d Opt i mi zat i on A ch ecki n g of spect romet er I n trod u ct i on Tabl e To obtai n the best fu rn ace t ech n i q u e, l arl y fu rn ace the th e th e it part I n i ti al are is of u si n g sh al l g raph i te parti cu - be opt i mi zed certai n u sed I S0 th e setti n g s, opti mi zed , meet s before rel evan t A wh en i n st ru men t setti n g s i n stru men t q u i remen t s the resu l ts the prog ramme, i n st ru men t th at in cri teri a performan ce in it is met h od - Pro g ramme for g raph i t e t u be d i ti on i n g On ce essen ti al perf orman ce the A re- speci fi ed 1 437 i n st ru men t ch e cks an d ad j u s t men t s A Swi t ch su ppl i es an d 2 Ope n tacts, or on f u me the power, fu rn ace Repl ace t ami n at i on th e extracti on the is cool i n g water, g as syst em an d i n spect g raph i te evi d en t th e t u be compon en t s I n spect the an d if A Spect romet er wi n d ows an d A cl ean if Wavel en g t h n ecessary I f a n ew t u be or g raph i te t h ese u si n g by man u fact u rer th e the t acts h eati n g are fi tted, prog ramme d i ti on reco mmen d ed Sel ect the of 1 437 I S0 A N OTE In the ommen d at i on s, i n tabl eA absen ce the sh ou l d of d i ti on i n g be the man u fact u rer’ s fu rn ace pro g ramme s h o wn u sed Rad i at i on Bot h Sel ect sh ou l d th e be i n stal l ed After th e th e are operat ed as l amps su i tabl e by (i e n ot by peri od th e or is 0, t h an mi n i n d i cati ve Th e sl i t wi d t h t wo t ype rel evan t part recommen d ed sl i t setti n g s provi d ed for by are u se wi th th e man u f ac- avai l abl e, the en su re g raph i te fu r- sel ected A by Backg rou n d A % f rom 0, 002 a fau l ty the sou rce th e man u f acsh ou l d maxi mu m absorban ce Si g n i fi can tl y of by radi ati on g reat er u n i ts) n ot correcti on Deu t eri u m val u e over fl u ctu ati on s Sel ect the l amps to of th e radi ati on backg rou n d correcti on u se of backg rou n d stabi l i ze an al yte for rad i ati on sou rce reco mmen d ed correcti on 30 are by th e mi n opti on Ch eck sou rce bal an ced an d wi th i n an d th at al l ow the the en erg i es th e d eu t eri u m th e tol eran ces man u fact u rer l amp A N OTE the Th es e reco mmen d ed speci fi ed each t h an mo re t i me f rom mo re of u su al l y in syst ems warm- u p si g n al devi ate are cat h od e l amps man u factu rer tu rer, a an d the Wh ere n ace h ol l ow d i sch arg e speci fi ed Sl i t tu rer so u rce si n g l e- el emen t el ectrod el ess wavel en g t h rec- th at A paramet ers wear mu l ti - el emen t l amps i s n ot Zee man backg rou n d correcti on syst ems g en eral l y recommen d ed En su re th at th e pol es of th e mag n et are cl ean I S0 1 437- : 994( E) A 3 Test of backg rou n d correcti on A syst em Wh e n pl atform, Measu re 20 a pl th e of a at omi c 0, % wavel en g t h 223, l an n m) u si n g 00 a ch arri n g atomi zati on u n d er backg rou n d mag n es i u m ( m/V) bet ween backg rou n d or an d nm sh ou l d correcti on of n i trate an d of be th e at omi c nm of 800 950 “C A wi th Bi an d l arg e no preven t i n g over Th e fi rst sh ou l d In be abl e absorban ces syst ems of to th e “C in 80 “C for cope for to wi th correcti on broad ban d absorban ce l evel s as Parti cu l ar the to I,0 ti p au t osampl er sh ou l d an d be the deposi ti on sh ou l d pai d to posi ti on Th e be th e of ch ecked d i ti on the ti p man u fact u rer’ s is of be the ad j u st men t of the th e L’ vov ben efi ci al in the h ol d i n g ti me Th e mai n t n ed ti me at i n j ected sampl e th e d u ri n g 80 Th e rapi dl y to t emperat u re “C at wh i ch d epen d s fol l owi n g th e on h ol d th e t i mes vol u me, ~1 H ol d ti me, s of d u ri n g 1 40 30 t emperat u re s to 30 s, boi l i n g poi n t is for h el d sampl e is to of t h en a th e s 20 sol ven t to i n j ected i n creased val u e 40 Th e s “C over to Th i s 40 h i g h er d epen d i n g fol l owi n g a “C on h ol d peri od above of th e t emperat u re th e t i mes vol u me are of typi cal i n stru cti on s au t osampl er vol u me, ~1 H ol d ti me, s sh ou l d fol l owed A Opt i mi zat i on of the f u rn ace A In d i ti on s Opti mi zat i on essen ti al of if g oo d tech n i q u e compl etel y u se wi th Th e sh al l th e in to to be n i ckel obt n ed the al l oy u si n g reco mmen d ed wi th al l oys fu rn ace matri x in is th i s by to th e si sts atomi zati on n i ckel of an d fou r man n er for 20 “C For is peratu re t h en th e h ol d mos t sh ou l d at sampl es t i mes be th at vol u me are en su re th at wi th it on ce the the d proceed s su i tabl e d ryi n g of d ryi n g process a d en tal smoot h l y can mi rror wi th ou t th e - Do ch arri n g , n ot vi ew at omi zat i on th e or t u be di rectl y cl ean i n g d u ri n g steps al l oy matri x basi c steps: cl ean i n g Ch arri n g Du ri n g th i s dri ven off red u ct i on the step, an d of vol ati l e compon en t s precu rsor th e an al yt e format i on react i on s oxi d e of mat ri x of the to of the occu r, the refractory matri x for el emen t al oxi d es are exampl e state an d car- bi d es sati sfactory h el d vi su al l y A 2, sel ected , d e- Dryi n g A an d been spatteri n g an d A mon i t ored A for h ere be A h ave WARN I N G Con seq u en t l y, pro g ramme the 40 sampl es A pro g ramme ch arri n g , to pro g ramme cern ed opti mi ze si d ered d ryi n g , often n i ckel A are h eat i n g pro g rammes are fu rn ace bei n g resu l ts u n rel ated an al yst scri bed fu rn ace Fu rn ace man u fact u rers th e the 40 h eat i n g pro g ramme on h eat i n g t h en sol u ti on I n j ected reg ard i n g an d sh ort I,5 Th e th e atten ti on pi pette sampl e a I n j ected 20 of i n vol ves s u n i ts operat i on is Ze eman Au t o s ampl er Th e on process typi cal backg rou n d as d eposi t ed syst em u n i ts hi gh t emperat u re vol u me si g n al d eu t eri u m correct u p to sh ou l d absorban ce A g en eral , are d ryi n g spatteri n g st ag e 80 are N OTE sampl es t wo- st ag e at ( e g “C observed , of sol u ti on 250 t emperat u re t emperat u re si g n al absorban ces a I S0 To a i n creased t emperat u re of sampl e d ryi n g avoi d t emperat u re spatteri n g , to 20 for a i n trod u ced “C th e in t i me 20 of t em- s Becau se mos t fol l owi n g Th e an al yst g raph i te i t wi l l sh al l tu be, measu ri n g typi cal of l ow remai n vol ati l i ty i n the of the fu rn ace after n i ckel al l oy ch arri n g an d d epen d i n g Th e N OTE matri x, fi rst n ormal mod e, peak sel ect or h ei g h t th e L’ vov or combi n at i on pl atform, peak area of an d to be u sed I n j ected vol u me, ~1 H ol d ti me, s Th e IO 40 30 an al yst ch arri n g A sh al l t emperat u re to A t h en d et ermi n e experi men tal l y th e as opt i mu m d escri bed in I S0 I S0 A Use t ermi n ed in the opt i mu m d ryi n g d i ti on s as d e- N OTE A Sh ort N OTE At at omi z at i on thi s s t ag e, set t i n g s at omi z at i on di t i on s bo t h are set t i n g s opt i mi z ed th e o pt i mu m u n kn o wn sh ou l d be ch arri n g Est i mat es m ad e an d f or the an d i n creas e t u be cau s e d S TOP ti me of an al yte IO s an d A Sel ect Th i s wi l l ch arri n g a a 30 co n - Sel ect th e i n teg rati on A wh ol e of cal i brati on read i n g Vary “C, taki n g the of compri si n g sol u ti on 0, ch arri n g t h rou g h ou t th ree ( A 4) at mat ri x at o ms the to a 30 s i n- wh i ch wi l l temperatu re, 500 for the me an each th e in “C st eps to cal i brati on of the of 40 “C sol u ti on t h ree t emperat u re ch arri n g N ot e absorban ce to N OTE starts obtai n th e to th e t emperat u re d ecl i n e to at Su btract opt i mu m 50 “C Pl ot th e in the is Use in s to men t s for s step Mon i t or cess N ot e ret u rn s in the to opt i mu m an d vary “C st eps of cal i brati on the the of th e h ol d s the at t i me Take sol u ti on backg rou n d t i me th e s ame f rom measu remen t s l oss ( i n d i cated ti mes) n al to A repeat If th e in sh al l f rom the ( A 4) th e of abs e n t g as eou s far to as an al yte is possi bl e, mi n i mi ze i n t er- STOP, mo d e combi n at i on ch arri n g the o pt i mu m g raph i te sel ect ed atomi zati on experi men t al l y t u be an d before the u si n g measu ri n g opti mi zati on step Al t h o u g h u si n g i ts ful l at omi zat i on q u i red ( STPF) in th e th e a opt i mi ze man n e r t h at In d i t i on s the d i t i on s Pl at f orm ad d i t i on to opt i mi ze the ( i n h eren t L’ vo v mod e sh ou l d Te mperat u re sat i sfi ed the me as u re me n t an al ys t mod i fi cat i on ad d i t i on al to h ei g h t s u ch are mat ri x fol l owi n g poss i bl e St abi l i zed o perat i on an d is pe ak pot en t i al , s t ep f or it the re- Fu r n ace to the u se in th e pro ced u re) , sh ou l d be of G AS sat i sfi ed Th e a t emperat u re an d the d i f f eren ce at omi zat i on t h an 000 s t ep “ C) be t we e n sh ou l d Th i s be al l ows th e as ch arri n g smal l th e as s t ep pos si bl e th i s pro ach d i t i on s q u i ckl y, an d wh i ch r ed u ce s th e ar e n earl y f u rn ace to amo u n t of i sot h ermal ap- mat ri x mo r e vol ati l i zed an y be p e ak ar e a i n t eg rat i on me as u r e me n t mod e sh ou l d u s ed sh al l be z e ro at omi zat i on t i me i n crease be t we e n th e ch arri n g st eps t emperat u re over th e ran g e measu re- d u ri n g d u ri n g A U se d i ti on s the opt i mu m d et ermi n ed in A d ryi n g an d an d A 2, ch arri n g - respecti vel y each th i s backg rou n d be in is no th ree pro- si g n al to 50 in A 8 l ess of an al yt e the A 20 Sel ect “C an d an an at omi zat i on i n teg rati on t i me t emperat u re of 20 of s i s sati sfi ed, backg rou n d Ad d is n ot u si n g t h an th at a U si n g ( A 41 , th i s th e obt n s ame t h ree atomi zat i on cal i brati on absorban ce sol u ti on measu remen t s at temperat u re l on g er s to si g - A Vary creasi n g it the st ep th e up to absorban ce as of d i rected atomi zati on in 000 the “C in t emperat u re 00 cal i brati on “C st eps sol u ti on by i n- Meas u re d u ri n g each A 3 th i s ti me A “C for the ( A 7) h ol d absorban ce evi d en ce in wh i ch opt i mu m A the d i ti on t i me d i ti on wh i ch of absorban ces basel i n e th e the act i on s t emperat u re sel ected to obtai n mean l ower th e sh ortest retu rn s val u e by Provi d ed the the Th ere h ol d sel ect is t emperat u re t h ree si g n al wh i ch G AS of A 3 A s ampl e s occu r basel i n e Cal cu l ate A 30 to th e acco mmo d at e ch arri n g th e be th e Th ere th e A 6 60 of As t i me an d fou n d sh ou l d tu be d et ermi n e s ys t em A of temperatu re to wo rki n g prod u ct i on g raph i te i n teg rati on me an wh i ch 50 ch arri n g al l o wan ce vari at i on s me as u ri n g t i me react i on s measu re- step t emperat u re the th e an d Th e Th e d ay- t o - d ay h ol d l oss sh al l ( l ess val u e pr o vo ke an al yst STOP the for rel ati n g absorban ce a spl at t er temperat u re N OTE step attai n ed g raph an d g i ve 0, ran g e meas u remen t s each Cal cu l ate men t s s th e th e A 6 may expl osi ve i n vol ves i n si d e Th e t i me st ep at o ms ach i eve 00 30 pret reat men t At omi z at i on pl at f orm A t i mes by of al l feren ce h ol d a absorban ce the set Sel ect atomi zati on th at an d measu red ch arri n g s l i teratu re accord i n g l y an en su res be Sel ect crease man u fact u rer’ s t emperat u re opti on peak A an th e at omi zati on G AS t i me f or su i t abl e Th i s th e sl ow su ffi ci en t fi rst Con su l t A 2 A u su al l y 1 43 7- : 9 4( E) sati sfi ed, A Pl ot obt n ed for the me an each st ep of the ag n st th ree th e meas u remen t s at omi zat i on t em- peratu re ch arri n g ori g i n al l y A 6 I S0 1 43 7- : 994( E) A est Exami n e th e atomi zati on abso rban ce obtai n is th e g raph an d d etermi n e temperatu re obtai n ed o pti mu m Ad d th e wh ere 200 atomi zati on “C l ow- m axi m u m to th i s val u e A Determi n ati o n of ch aracteri sti c I S0 m ass, to temperatu re A u ti on Measu re Sl th ree th e absorban ce ti mes, u si n g th e of cal i brati on i n j ecti on sol - vo l u me rec- N OTE S o mme n d e d IO At mu m th e l o west atomi zati on abso rban ce measu remen t wh e n mo d e, tai l i n g Th e extra 1 th e L’ vo v th e th e peak g i vi n g area peaks are broad wi th “C wi l l 200 temperatu re u si n g o verco me th ese maxi - - abso rban ce d i ti on s, ch e ck ch arri n g pl atform th at th e temperatu re is to be u sed d i fferen ce an d si d erabl e probl ems u n d er between o pti mi zed A u ti on Measu re S2 th ree STP F - th e d o es n ot exceed 00 - absorban ce proced u re Cal cu l ate th e me an th e absorban ce ti mes, in th e u si n g th e of cal i brati on i n j ecti on proced u re sol - vo l u me Cal cu l ate th e recme an A, , o pti mu m atomi zati on temperaA tu re th e i n teg rati on o mme n d e d If in As, Th e ch aracteri sti c m, mass, is g i ven by th e in cal i - “C eq u ati on : A Du rati on of th e atomi zati on step p x m, = U se th e h ol d o pti mu m ti me of temperatu re fou n d in A an d v x 0, 004 ‘ 4s2 a - 41 s wh ere i n stru men ts eq u i pped wi th a VD U or is P fast record er th e cen trati on brati on n an og rams Measu re th e th e ato mi c termi n e ti me th e cal i brati on si g n al th e o pti mu m taken for th e absorban ce A sol u ti on d u ri n g th e h ol d trace ( A 4) ti me to an d atomi zati on by retu rn to th e s De- to V is th e zero- axi s a VD U or fast th e vo l u me pressed A wi th ou t an al yte expressed in mi l l i l i tre; in of th e sol u ti on i n j ected , ex- mi crol i tres of scal e I n stru men ts per th e S2 , observe stag e ad d i n g of sol u ti on Determi n ati o n of mi n i mu m preci si o n reA Measu re th e absorban ce of cal i brati on sol - cord er u ti on M ake th ree u sed in measu remen ts A peat th ese h ol d ti mes Cal cu l ate (1 s at th i s A H eat poi n t to Cl ean i n g th e m u ch of u n ti l th e absorban ce prog ressi vel y th e d ecrease obtai n sol u ti on me an Ad d of sh orter th e s to o pti mu m Re- o mme n d e d i n d i vi d u al me an refractory at resi d u al In 650 “C for matri x as possi bl e mo ve d , A practi ce, h ol d A even at an d hi gh ti me s to remo ve fol l owi n g u si n g tabl e of th e of tests th e th e matri x carbi d es A el emen ts can n ot be proced u re read i n g s th e S2 A, , stan d ard u si n g Cal cu l ate th at sol u ti on an d rec- Reco rd th e cal cu l ate th e th e d evi ati on sa for cal i - eq u ati on sh al l be rel evan t re- of mi n i mu m u si n g th e preci si on for cal i - formu l a 00 - A cri teri a performed d escri bed sol u ti on s part th e S2 fo rm compl etel y Measu re I S0 in after A i d en ti fi ed to in opti A 6, , j ecti on Reco rd cu l ate th e cal i brati on vo l u me th e th e ten re co mmen d ed i n d i vi d u al me an absorban ce sol u ti on absorban ce val u e of th e ti mes, in mo st u si n g th e read i n g s - th e i n- proced u re A, an d cal - for th e & 1 43 mo st Cal cu l ate cen trated eq u ati on vo l u me 42 pe rfo rman ce i n stru men ts cal i brati on th e rel evan t i n j ecti on as temperatu res I n stru men t mi zati on th e A, , sol u ti on cen trated Th e th e Cal cu l ate brati on SBx o xi d es in u si n g abso rban ce val u e brati on N OTE ti mes, th ree th e h ol d ten step fu rn ace th e to cal i brati on mean u si n g i n terval s) starts th e th e measu remen ts measu remen ts ti me of S2 th e stan d ard cal i brati on d evi ati on sol u ti on u si n g th e I S0 I S0 A s* = pq G - Cal cu l ate pi cog rams, u si n g th e th e l i mi t of 1 43 7- : 9 4( E) d etecti on %i ”, in eq u ati on pxVxsBxK Si n = A mo st Cal cu l ate th e cen trated mi n i mu m cal i brati on preci si on sol u ti on u si n g for th e th e for- As2 - - AS1 wh ere mu l a s, x 00 is P th e cen trati on brati on A, sol u ti on n an o g rams A De termi n ati o n d etecti on , A u ti on of th e l i mi t of V is mmi n ten o mmen d e d th e ti mes, in absorban ce - absorban ce u si n g th e th e proced u re read i n g s As, an d of cal i brati on i n j ecti on vo l u me Reco rd cal cu l ate th e th e i n d i vi d u al me an K sol - is A Measu re ten o mme n d e d abso rban ce - th e ti mes, in abso rban ce u si n g th e th e proced u re read i n g s AS2 an d of cal i brati on i n j ecti on Reco rd cal cu l ate vo l u me th e th e sol rec- th ree val u e A brati on sol u ti on S= B J c ( 42 S2 u si n g stan d ard th e d evi ati on eq u ati on of th e sol u ti on as g raph i n j ected , ex- l i n eari ty in th e wh o l e u si n g set th e of cal i brati on sol - vo l u me rec- i n j ecti on proced u re abso rban ces ss for m ass a Cal cu l ate obtai n ed g raph of vo l u me for each th e me an of sol u ti on th e of rel ati n g an al yte, th e th e in cal i brati on me an abso rban ces n an o g rams, in th e i n- sol u ti on s cal i A Obtai n spon d i n g &2 ) in mi l l i l i tre; taken th e ti mes Pl ot th e j ected th e S2 , mi crol i tres; for Measu re th ree o mme n d e d th e to Cal cu l ate cal i - i n d i vi d u al me an 42 A in n ormal l y Cri teri on u ti on s S2 vo l u me in expressed val u e A u ti on per an al yte rec- 41 A th e pressed Measu re Sl of an d th e bo tto m to n et 20 A 4 Th i s rati o th e th e top n et 20 absorban ce % of th e Cal cu l ate sh al l n ot abso rban ce % of val u e covered th e be rati o l ess th e A, val u e covered AA m ass correspon d i n g m ass correran g e to th e ran g e AA/A, th an I S0 CJ I S0 1 437- : 994( E) An n e x B ( i n formati ve) Exampl es Th e exampl es of composi t i on s of g i ven composi t i on s in tabl e B l are n ot of to be s o me i n terpreted n i ckel as al l oys speci fi cati on s for ch emi cal co mpo - si ti on s Tabl e Si n g l e val u es are B l maxi mu m Exampl es - l i mi ts, of except composi t i on s for n i ckel , wh ere of s o me si n g l e n i ckel val u es are al l oys [% ( m/m) ] mi n i mu m - 0 - 4, 0 , 00 0 - - - 0, 08 - 9, - 23 , I,0 0, 02 0, J L 8, 21 , 0, 00 4, 0, 0 2 0, 05 K 21 04 9, 0 21 21 , 0, 02 1 , 03 0, 2 0, 01 0 1 21 , 0, 2 4, I Al l oy 2) Wh e r e rn h al t l etters no are l i mi t s rn l wWc as u sed are i n st ead g i ven , n i ckel in of th e so me 70, 03) comme rci al m axi m u m al l n vs n am e s cobal t - 0, 5 Re- - mai n d e r 0, 5 0, o 3 5 0 01 0, 5 - 0 - - - - I,0 - Re m n - - 0, 01 - 1 0 0 - Re mai n - Re mai n - 5 d er Re mai n - - 1 - u n ti l t en t a is n eu t ral % I S0 2 , 20 - 60 d es i g n at i on ( m/m) Re m n d er3) Re mai n - d er Re mai n - d er is d eve l ope d Ot h ers Nb - 0, 01 - - 0, 01 , 07 0 0, 40 0, 0, 01 0, 01 Nb 0, 08 Ta to pl u s to Ta 55 - Pb 0, 00 Zr 0 Zr 5 Ti 4 pl u s - to Al - 3 0, 040 pl u s d er 30 0 d er Ti d er3) 2 Re- 6, I) - 21 I mai n d er 8, O H 21 , 0 60 G 7, Of F 7, o Si Zr 0 - v w to 08 to I S0 I CS 1 43 7- : 9 4( E) 77 20 40 De scri pto rs: n i cke l al l oys, g en eral i ti es Pri ce based on pag es ch e m i cal an al ysi s, d etermi n ati on of ten t, trace el eme n ts, ato m i c absorpti on spe ctrome tri c meth od ,