BS 6068-2 29-1987 Water quality - Physical chemical and biochemical methods - Determination of cobalt nickel copper zinc cadmium and lead flame atomic absorption spectrometric meth.pdf

1、BRITISH STANDARD BS 6068-2 . 2 9 :1987ISO 8 2 88: 1986Wat er q u a lity Par t 2:Ph ysi cal ,chemical a ndb ioc hemicalme t hods S e c t ion 2 . 2 9 D e t ermin a t ionof c o bal t ,nic kel,copper, zinc,cadmiu m a nd lea d :fla me a t omicab s orpt ion s pec t romet ricmet hods ISO ti t le:Wa t er q

2、u a lity D e t ermina t ionofc o bal t , nic kel,copper,z inc,cadmi u m a ndlea dF l a mea t omi cabs orp t ion spec t romet ric met hod s ICS: 13.060.50IncorporatingCorrigendum No. 1BS 6068-2 . 2 9 : 1987T his B rit i s h S t a nda rd, h a v ingb eenprepa red u nder thedire c t ionof the E n v iron

3、ment a nd P ollution S t a nda rds C ommittee, wa s p u b lis hedu nder t hea uthority of theB o a rdof BSI a nd c omesint oeffec t on27 F e b r u a r y 1987T hefollow ing BSI referenc e s rela t e to the workon this sta nda rd:C ommitteereferen c e EPC / 44D r a f t for c omment 85/ 5 0076 DCA md.

4、N o. Dat eofissue C omments The British StandardsInstitution 2015. Published byBSI Standards Limited 2015ISBN 978 0 580 92292 3Amendments/corrigenda issued since publicationC1 December 2015 Supersession information updated.BS 6068-2 . 2 9 : 1987iC ont entsPageNat iona lforew ord ii1 Scope 12 F ieldo

5、f a pplicat ion 1S e c t ion1. M e t hod A D ire c t det ermin a t ion b y fla me a t omi cabs orp t ion spec t romet r y3 P rinc iple 24 R e a gents 25 A ppa r a tus 26 Samplinga nd sa mples27 P roc edu re 28 E x pressionofresul ts 39 T e st report3S e c t ion 2. M e t hodB D e t ermina t ionb y fl

6、a mea t omicab s orpt ions pec t romet r y a f t er c hela t ion( APDC) a nde xtr act ion( MIBK)1 0 P rinc iple 411 R e a gents 41 2 A ppa r a tus 41 3 Samplinga nd sa mples 414 P roc edu re 415 E x pressionofresul ts 51 6 T e st report 5S e c t ion 3. M e t hodC D e t ermina t ionb y fla mea t omic

7、ab s orpt ions pec t romet r y a f t er c hela t ion( HMA- HMDC) a nde xtr act ion( DIPK- xylene)1 7 P rinc iple 718 R e a gents 719 A ppa r a tus 720 Samplinga nd sa mples72 1 P roc edu re 722 E x pressionofresul ts 823 T e st report 9A nnex APret rea t ment of the sa mple whendet ermining to t a l

8、me t a l s 1 0A nnex BChec kingc omplet eextr act ion( M e t hodC )10Table11Table 2 1Table 3 1Table4 3Table5 3Table 6 5Table 7 6Table89 The British Standards Institution 2015BS 6068-2 . 2 9 : 1987iiNat iona lforew ordT his S e c t ionof BS 606 8 , whic hha s b eenprep a red under thedirec t ionof th

9、eE n v ironment a nd P oll ution S t a nda rds C ommittee, i s ident i cal wi t hISO 8 2 88-1986 “ Wat er q u a lity D e t ermina t ion of c o bal t , nic kel,copper, zinc,cadmi u m a nd lea dF l a me a t omi cab s orpt ion spec t romet ric met hods ”. T heint erna t iona l st a nda rd wa s prepa re

10、db y subcommittee 2 ,Ph ysi cal ,chemical a ndb ioc hemicalme t hods , ofT e c hnical C ommittee147 ,Wa t erq u a lity, of theI n t erna t iona l O rga niz a t ionforS t a nda rdiz a t ion( ISO) a s a resul t ofdis c ussioninw hic h the UK p a r t i c ipa t ed.T his B rit i s h S t a nda rdi s b ein

11、gp u b lis hedin a series ofPar ts sub div idedint oS e c t ion s th a t w illgenera lly c orres pond topa r t i c u l a rin t erna t iona l st a nda rds .S e c t ions a reb eing, or willb e , p u b lis hedinPar ts 1 to 6 , whic h toget her wi t hPar t0,arelistedb elow . Par t0:In t rodu c t ion; Pa

12、r t 1 :Glossa r y; Par t2:Ph ysi cal ,chemical a nd b ioc hemicalme t hods; Par t3:Ra diologicalme t hods; Par t 4 :Mi c rob iologicalme t hods; Par t 5 :Biologicalme t hods; Par t6:Sa mpling.T erminolog y a nd c onv ent ion s . T he te xt of theint erna t iona l sta nda rdh a s b eena pprov eda s s

13、ui t ableforp u b licat iona s aBrit i s h S t a nda rd wi t hout dev i a t ion. S ome terminology a ndc ert a inc onv ent ions a renot ident i cal wi t h thos eusedinB rit i s h S t a nda rds; a ttent ioni s dra w nes pec i a lly t o thefollow ing.T hec omma h a s b een us eda s a dec ima lma rker.

14、I n B rit i s h S t a nda rds i t i s c u rrent pract i c e to us e a f u llpoint on thebas elinea s t hedec ima lma rker.I n B rit i s h S t a nda rds i t i s c u rrent pract i c e to us e the sy m b ol“ L ”forlit re( a ndini ts sub m u l t iples )ra t her th a n“l”,and to us e the spelling“ sulphu

15、 r”, e t c ., inste a dof“ sulfu r”, e t c .W herev er the words “ t his I n t erna t iona l S t a nda rd”a ppea r , referring to this sta nda rd, they s hou ldb ere a d a s “ t his S e c t ionof this B rit i s h S t a nda rd”.NOTE T y pogra phi calerror s . I n 18.6 , p a r a gra ph1 , line1 ,andp

16、a r a gra ph 3 , line1 , “ s olutions ”s hou ldb ere a d a s “ s olution”.I n 22. 3 , p a r a gra ph 3 , line1 , “neutr a l” shou ld b ere a d a s “na tur a l”.contract.Users areresponsiblefor itscorrect application.Compliance with a British Standard cannot confer immunity fromlegal obligations.S u

17、mma r y of p a gesT his doc u ment c ompris e s a front c o v er,anin s idefront c o v er, p a ges i a ndii,p a ges 1 to10 a nd aback c o v er.T his sta nda rdh a s b een upda t ed( s eec opy right d a t e)a ndm a y h a v eha da mendments inc orpora t ed. T his w illb eindicat edin thea mendment t a

18、bleon theins idefron t c o v er.Thispublicationdoes not purport toincludeall thenecessary provisions ofaThis Section of BS 6068 is published by BSI Standards Limited, under licence from The British Standards Institution.This Section of BS 6068 partially supersedes BS 2690-1:1964 which is withdrawn.

19、The British Standards Institution 2015BS 6068-2 . 2 9 : 198711 ScopeT his I n t erna t iona l S t a nda rd spec ifies t hreemet hod s for thedet ermina t ionofc o bal t , nic kel,c opper, z inc, cadmi u m a ndlea din wa t erb y fla mea t omicab s orpt ion spec t romet r y :S e c t ion 1 : met hodA,f

20、ordirec t det ermina t ionb y fla mea t omi cab s orp t ion spec t romet r y;S e c t ion 2: met hodB,fordet ermina t ionb y fla mea t omicab s orpt ion spec t romet r y a f t erc hela t ion( APDC) a nde xtr act ion( MIBK) ;S e c t ion 3: met hodC,fordet ermina t ionb y fla mea t omicab s orpt ion sp

21、ec t romet r y a f t erc hela t ion( HMA- HMDC) a nde xtr act ion( DIPK- xylene).2 F ield of a pplicat ion2 .1 M e t hod A i s p a r t i c u l a rly a pplicable whenc onc ent r a t ions ofelements t o b e a n a l ysed a rerela t i v ely high a nd when therea renoint erferenc e s .W hen the sa mples

22、a reof acomplex or unknow nn a tureor when they c ont a inhighc onc ent r a t ions ofdissolv ed solids ( b rines or b r ackis h wa t ers )met hodA i s not a pplicablea ndeit hermet hodB orCs hou ldb e selec t ed.T hec onc ent r a t ion s ofelements whic h can b edet erminedb y met hodA m a y v a r y

23、 according to thec h a r act eri sti c s of thea t omicab s orpt ions pec t romet ricappa r a tus usedb ut a regenera lly int her a nge s indicat edin Table1.Table 1I f thec onc ent r a t ions a regrea t er th a n the upperlimits indicat edin the table, the sa mplem a y b edilutedb eforea n a l ysi

24、s .2 . 2 M e t hod s BandCarea pplicable whenc onc ent r a t ion s ofelements to b e a n a l ysedin thes a mple(ordilutionof the sa mple)a regrea t ert h a n 0 ,5 4 g / l.2 . 2 .1 M e t hod BT hec onc ent r a t ions of theelements w hic h can b edet erminedb y met hodB m a y v a r y according to the

25、c h a r act eristi c s of t hea t omicab s orp t ions pec t rome t er us edb ut a regenera lly in ther a nges indi cat edinTable 2.Table 2 2 . 2 . 2 M e t hod CW i t h a r a t ioof te st port ion t oextr act ion solutionof 20 t o1b y v olu me a s indicat edin 2 1.2 , thec onc ent r a t ion s ofeleme

26、nts w hic h can b ede t erminedb y met hodC va r y a s indicat edinTable 3.Table 3 L o w erc onc ent r a t ions m a y b ede t erminedb y c hoos ing a higherr a t ioof te st port ion toextr act ions olution.A r a t ioof5 0 t o1b y v olu mei s possi b les inc e theorg a nic solv ent mixtu rei s onl y

27、v erys light l y s olu b lein wa t er.W i t hme t hodC, sepa r a t ionof thea q u eous a nd theorga nic pha s e s i s f a ster.T hemet a l c hela t e s ,e s pec i a lly t heC d-c hel a t e ,aremore stablein theorga nic solv ent mixture.NOTE1 W hendet ermining to t a lme t a l s , i t i s nec e ssa r

28、 y topre t rea t t he sa mpleb eforea n a l ysi s ( s eee x a mples ofproc edu res inA nne x A ).NOTE 2 M e t hods BandCarenot a pplicable when thec hemicalo xygendema nd( COD )of the sa mples (ordiluted sa mples )is gre a t er th a n500 mg/ l.E lement t o b ede t ermined Rangeofde t ermina t ion(mg

29、/ l)C o bal tN i c kelC opperZ incCadmiu mL e a d0 ,1 to100 ,1 to100 , 0 5 to 60 , 0 5 to 20 , 02 t o 20 , 2 t o10E lement t o b ede t ermined Rangeofde t ermina t ion( 4 g / l)C o bal tN i c kelC opperZ incCadmiu mL e a d1 t o 2001 t o 2001 t o 2000 , 5 to500 , 5 to505 t o 200E lement t o b ede t e

30、rmined Rangeofde t ermina t ion( 4 g / l)C o bal tN i c kelC opperZ incCadmiu mL e a d0 , 5 to1000 , 5 to1000 , 5 to1000 , 2 t o500 , 2 t o502to 200 The British Standards Institution 2015BS 6068-2 . 2 9 : 19872S e c t ion 1. M e t hod A D irec t det ermina t ion b y fla me a t omi cab s orp t ion sp

31、ec t romet r y3 P rinc ipleA s pira t ionint o thefla meof a n a t omicab s orpt ions pec t romet erofa te st port ionof theacidifiedfilt r a t eof the sa mple(ordiluted sa mple).D ire c t det ermina t ionof thec onc ent r a t ionofe achelement , eit herfrom the spec ificab s orban c eofeachelement

32、using a spec t romet erfitted wi t h ac ont inu o us backgrou ndc orre c t ion system, or, in theabs enc eof su c h a system,af t erh a v ingcarriedo ut ac orrec t ionfor a non- s pec ifi cab s orban c e.4 R e a gentsA llrea gents s h a llb eofre c ogniz eda n a l yti calgr a des o th a t t heir us

33、edoes not a ffec t t heaccu r acy of thedet ermina t ion.T he wa t er us ed sh a llb edeioniz edw a t erordistilled wa t erc ont a iningnodet e c t ablec onc ent r a t ionof themet a l s b eingdet ermined whena n a l ysed b y abl a nk te st.4.1 N i t ricac id, A =1,4g/ ml.4.2 N i t ricac id, c ( HNO

34、3 ) 1 ,5mol/ l.A dd1 00 mlofnit ricac id( 4.1) to 600 mlof wa t era nddilute to1000 ml.4.3 N i t ricac id, c ( HNO3 ) 0 , 03 mol/ l.A dd1mlofni t ricac id( 4.1) to400 mlof wa t er a nddilute to500 ml wi t h wa t er.4.4 M e t a l s , sta nda rd solutions c orres pondingt o1, 000 gofme t a lperlit re.

35、1)F ore achelemen t t o b ede t ermined , weigh1 , 000 gofp u remet a l a nddissolv eit innit ricac id( 4.1) ,hea t ing toeffec t c omplet edi ssolution.A llow t o c oola nd tr a n s fereach solutionqu a n t i t a t i v ely t oa 1 000 mlone-ma rk volu met ric fla s k , dilute to them a rk wi t h wa

36、t era ndmix .F orprepa ring st a nda rd solutions , i t i s a l s opermissi b le to us eme t a l sa l ts ofaccu r a t ely know nc ompos i t ion.S t oreeachof the sta nda rd solution s ineit herpoly e t h y leneorb oro s ili cat egl a ss c ont a iner s .1mlofeachof thes e st a nda rd solutions c ont

37、a ins 1 , 00 mgof theres pec t i v eme t a l.5 A ppa r a tusU sua llabora t ory equ ipment ,andA t omicab s orpt ion spec t romet er, fitted wi t hhollowcat hodela mps for thea ppropria t eme t a l s orelec t rodele ss dis c h a rgel a mps ,and wi t h a su i t abledev i c efora llo w ingfor the c or

38、rec t ionof thenon-s pec ifi cab s orban c e a nd wi t h a neb u liz erb u rnerw i t h a n ace tylene- a irfla me.F ollow t hem a n u f acturers instr u c t ions fora djustinga llinstr u ment p a r a met ers .NOTE ON CLEANING OF GLASSWAREA ll thegla sswa re sh a llb e carefu lly s o a kedinnit ricac

39、id( 4.2 ) thenrins ed wi t h wa t er.6 Sampling a nd sa mples6 .1 P oly e t h y leneorb oro s ili cat egl a ss c ont a inersw hic hha v e b eenprev iousl y c lea ned wi t hni t ricacid( 4.2 ) thenrins ed wi t h wa t er, sh a llb e us edfors a mpling.6 . 2 I f to t a lme t a l s a re to b ede t ermin

40、ed, sa mples s h a llb e trea t ed b y t hea ddi t ionofni t ricac id( 4.1)immedia t ely a f t erc ollec t ioninorder toob t a ina p Hb e tween1a nd 2 ( usua lly2mlofacidperlit reofs a mpleis suffic ient ).N o t e thea mou n t ofacida ddeda nd us e the sa me volu mein theprepa r a t ionof theb l a n

41、k( 7 . 2 ).I fonly dissolv edmet a l s a re to b ede t ermined, filt ert he sa mplea s soon a s possi b le a f t er c olle c t iont hrou gha memb r a nefilt erofnomin a lporedia met er 0 , 45 4 m a ndacidify thefilt r a t eimmedia t ely w i t hni t ricac id( 4.1)inorder toob t a ina p Hbe tween1 a n

42、d 2 .B efore use , filt ers sh a ll b e thorou ghly w a s hed wi t hnit ricac id( 4.2 ) a ndrins ed wi t h wa t er.7 P roc edu re7 .1 T e st port ionI n t o a 1 00 mlone-ma rk volu met ric fla s k , place at e st port ionof theacidified sa mple( 6 . 2 ) su c h th a t i t c ont a ins0, 2 t o1mgofme t

43、 a l(s eeTable1for theu pperlimits c orres ponding toeachelement ).Makeu p to them a rk wi t h wa t er.7 . 2 B l a nk te stCarry o ut abl a nk te st inp a r a llel wi t h thedet ermina t ion,by the sa meproc edu re, using thes a meq u a n t i t ies ofa ll therea gents a s in thes a mplinga nddet erm

44、ina t ion,but replacing the te st por t ion b y w a t er.7 . 3 P repa r a t ion of the se ts of calib r a t ions olutionsB eforee ach bat c hofde t ermina t ions , prepa refrome achof the sta nda rd solution s ( 4.4) a t lea st fou rcalib r a t ion solutions c o v ering, fore achelement , ther a nge

45、of t hec onc ent r a t ion s t o b ede t ermined.P repa re thes e calib r a t ion solutions b y dilutingsta nda rd solutions ( 4.4) wi t hni t ricac id( 4.3 ).1)S t a nda rd solutions a rec ommerc i a lly a v a ilable. The British Standards Institution 2015BS 6068-2 . 2 9 : 198737 .4 Calib r a t ion

46、 a nd det ermina t ionP roc eeda s follows fore achme t a l b eingdet ermined.B eforecarry ingout the spec t romet ricmea surements, se t u p the spec t romet eraccording tot hem a n u f acturers instr u c t ions b y a s pira t ingacalib r a t ion solution( 7 . 3 )of thep a r t i c u l a rme t a lb

47、eingdet ermineda nd using t heinforma t ioninTable4.O p t imiz e thea s pira t iona ndfla mec ondit ions ( a s pira t ionr a t e , n a tureof thefla me,pos i t ionof theopt i cal b e a min thefla me).A djust t heres pons eof theinstr u ment t o zeroabs orban c e wi t hw a t er.Table 4F ore achme t a

48、 l b eingdet ermined,as pira t e the se t ofcalib r a t ion solutions ( 7 . 3 ) a nd,as z eromemb er, theb l a nk solution( 7 . 2 ).P lot a gra phh a v ing themet a lc ont ents, inmilligr a m s perlit re, of thecalib r a t ions olutions a s abs c i ssa e a nd thec orres ponding va l u e s of abs orb

49、an c e a s ordin a t e s . I t i s a d v i s able th a t t hecalib r a t iongra ph b e c hec ked , fore x a mple b y mea suring the abs orban c eof aca lib r a t ion solutione v ery 5 sa mples .A s pir a t e the te st port ion( 7 .1)in t o thefla meof theb u rner.M e a sure the abs orban c eof themet a l b eingdet ermined a nda f t ere achme a suremen t a s pir a t et henit ricac id( 4.3 )inorder torins e theneb u liz ersystem.NOTE ON CORRECTION FORNON- SPECIFICABSORPTIONI f the spec t romet er us edi s not fitted wi t h abackgrou ndc orrec t ion system whic