IS 13963-1: Chemical analysis of cadmium metal, Part 1: Determination of copper, zinc, lead and iron

9 Pages·1994·1.2 MB·English

by  Bureau of Indian Standards

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IS 13963-1 (1994): Chemical analysis of cadmium metal, Part
1: Determination of copper, zinc, lead and iron [MTD 9:
Lead, Zinc, Cadmium, Tin, Antimony and their Alloys]
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IS13963(Pattl ):I993

YTTT 1
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Indian Standard
CHEMICALANALYSISOFCADMIUMMETAL
PART 1 DETERMINATION OF COPPER, ZINC, LEAD AND IRON
UDC 669’73 : 543 : 546’47’56’728’15

@ BIS 1994
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

February11994 Price:Grorp 2
sdohteU fo lacimehC sisylanA fo suorreF-noN Metals lanoitceS ;eettimmoC DTM 28
FOREWORD
sihT naidnI dradnatS was detpoda yb eht uaeruB fo naidnI Standards, retfa eht tfard dezilanif yb
eht sdchtem fo lacimehC sisylanA fo suorreF-noN lanoitceSslateM eettimmoC bad neeb devorppa
yb eht lacigrullateM gnireenignE noisiviD .licnuoC
1s 6344 : 1985 noitacificepS‘ rof muimdac ’slatem srevoc eht stnemeriuqer fo suoirav sedarg fo
this .lairetam ehT lanoitceS eettimmoC elbisnopser rof noitaraperp fo this standard dediced that
eht sdohtem fo lacimehc sisylana fo suoirav stneutitsnoc debircserp ni SI 6344 : 1985 yam eb
derevoc ni tnereffid parts fo eht standard. ylgnidroccA this standard ( traP 1 ) has neeb deraperp
ot ebircsed eht cimota noitprosba cirtemortceps dohtem rof noitanimreted fo ,reppoc ,cniz dael
and nori ni muimdac .latem ehT cirtemotohportceps dohtem rof noitanimreted fo reppoc and
nori and cihpargoralop dohtem rof noitanimreted fo cniz and dael evah osla neeb debircserp as
etanretla .sdohtem
ehT traP 2 fo this standard sebircsed eht cirtemotohportceps sdohtem rof noitanimreted fo ,lekcin
,cinesra ynomitna and muillaht ni muimdac .latem
nI gnitroper eht stluser fo tset ro sisylana edam ni ecnadrocca htiw this standard, fi eht lanif .,eulav
devresbo ro ,detaluclac is ot eb dednuor ,ffo ti shall eb enod ni ecnadrocca htiw SI 2 : 1960 seluR‘
rof gnidnuor ffo laciremun seulav ( desiver .‘)
IS 13963 ( Part 1) : 1994
Indian Standard
CHEMICAL ANALYSIS OF CADMIUM METAL
PART 1 DETERMINATION OF COPPER, ZINC, LEAD AND IRON
1 EPOCS 5.2.2 rof ,nZ Cu, ,bP
Hollow Cathode Lamps
and .eF
sihT star:dard ( traP 1 ) sebircsed cimota -prosba
noit cirtemortceps sdohtem rof noitanimreted
fo ,reppoc ,cniz dael land nori as eht eerefer 5.3 Reagents
.sdohtem tI osla sebircsed cirtemotohportceps
dohtem rof noitanimreted fo reppoc and nori 5.3.1 Hydrochloric acid, dr = 61’1 ( gnimrofnoc
and cihpargoralop dohtem rof noitanimreted fo ot SI 265 : 1993 )
cniz and dael as etanretla .sdohtem
5.3.2 dr = 24’1 ( gnimrofnoc ot
Nitric Acid,
2 SECNEREFER SI 264 : 1976 )
ehT gniwollof naidnI Standards era yrassecen
5.3.3 1 ,tnecrep 50 tnecrep
stcnujda ot this standard: Difuft? Nitric Acid,
( v/v )
SI .oN Title
264 : 1976 cirtiN dica ( second revision > 5.3.4 Dilute Hydrochloric Acid, 1 tnecrep ( v/v )
265 : 1993 cirolhcordyH dica ( fourth
5.3.5
revision > Standard Solutions
1817 : 1961 sdohteM fo sampling fo -non
suorref latem rof lacimehc 5.3.5.1 Standard copper solution ( 1OOppm )
sisylana
refsnarT 00’1 g fo reppoc ( ytirup 99’99 tnecrep
1070 : 1992 tnegaeR edarg retaw ( driht
nim ) ot a 250 lm rekaeb and add 15 lm fo etulid
revision ) cirtin dica ( 1 : 3 ), mraw yltneg litnu reppoc
.sevlossid ,looC add 20 lm retaw and liob
3 GNILPMAS
again. refsnarT eht noitulos ot 1 ertil cirtemulov
elpmaS shall eb drawn and deraperp ni -rocca Aask and ekam up. xiM .ylhguoroht ekaT 10 lm
ecnad htiw erudecorgeht laid nwod ni SI 6344 : fo this noitulos and etulid ot 100 .lm ( noituliD
1985 and SI 1817 : 1961. is enod as and nehw deriuqer .)
,4 YTILAUQ FO STNEGAER
5.3.5.2
Standard zinc solution ( 100 ppm )
Unless deificeps ,esiwrehto lacitylana edarg

stnegaer and dellitsid retaw ees( 1s 1070 : 1992 ) evlossiD 00’1 g fo cniz ( ytirup 99’99 tnecrep

shall eb deyolpme rof eht .tset nim ) ni 20 lm etulid cirolhcordyh dica ( 1 : 4 .)
etuliD ot 1 .ertil ekaT 10 lm fo this noitulos
,5 NOITANIMRETED FO ,REPPOC CNIZ and etulid ot 100 .lm ( noituliD is enod as and
DAEL AND IRON YB CIMOTA NOITPROSBA nehw deriuqer .)
CIRTEMORTCEPS. DOHTEM
5.1 eniltuO of the Method 5.3.5.3 Standard lead solutiow( 100 ppm )
The elpmas is desopmoced yb tnemtaert htiw evlossiD 00’1 g fo erup dael ni muminim emulov
cirolhcordyh dica and cirtin .dica ehT mass is fo cirtin dica and etulid ot 1 ertil htiw etulid
detaropave ot ypurys ycnetsisnoc and neht cirtin dica ( 1 tnecrep ) ro evlossid 895’1 g fo
devlossid ni .retaw ehT touqila is nekat ot dael etartin ni etulid cirtin dica ( 1 tnecrep ) and
erusaem ecnabrosba~eht fo ,reppoc ,cniz dael and etulid ot 1 ertil htiw etulid cirtin dica ( 1
,cadmium against standard noitulos gniniatnoc tnecrep 1. etuliD 10 lm fo this noitulos ot 100
all eht tcejbus stnemele at shtgnelevaw ,7’423 lm ( noituliD is enod as and nehw deriuqer .)
,9’312 9’712 and 3’842 mn .ylevitcepser
5.2 Apparatus 5.3.5.4 Standard iron solution ( 100 ppm )
5.2.1 ynA standard cimota noitprosba -ortceps
evlossiD 00’1 g fo erup nori ni 50 lm fo etulid
retemotohp htiw htgnelevaw egnar morf 200
ot.* 900 mn is elbatius ( ees etoN 1 .) cirtin dica ( 50 tnecrep .) etuliD to 1 ertil htiw
dellitsid .retaw etuliD 10 lm fo this noitulos ot
NOTE -l stnemurtsnI taht nac daer ni -artnecnoc 100 .lm ( noituliD is enod asand nehw -iuqer
noit edom dna htiw auto orez ytilicaf lliw eb fo
der .)
.egatnavda
1
IS 13963( Part 1 ) : 1994
NOTE 2 - ehT dohtem fo dradnats snoitidda yam
5.4 Standard Conditions for Determination of
eb dewollof ni esac cimota noitprosba retemortceps
,nZ Cu, Pb and Fe by Atomic Absorption nac yltcerid daer ni noitartnecnoc edom dna si
Spectrometer dedivorp htiw auto orez .ytilicaf
laeR elpmas noitulos B ni noitartnecnoc edom dna
Element Light Source Wavelength Slit Width tes eht cirtemotohp gnidaer ot orez yb gnisserped
( nm ) (nm) auto orez .hctiws nehT etaripsa eht ( elpmas +
cu wolloH edohtac 1’423 0.~7 dradnats1 mpp ( noitartnecnoc ) noitulos C dna fo tes dradnats eht noitartnecnoc dedda ni ksalf ot C
lamp
si lauqe ot 1.0 mpp .) daeR eht noitartnecnoc fo eht
nZ od 9’312 7’0 knalb .A nehT eht etulosba eulav fo eht evitagen
gnidaer deniatbo lliw dnopserroc ot eht -necnoc
bP od 0’712 7’0 noitart fo eht tnemele ni eht elpmas .noitulos
eF od 3’842 2’0 ,tnemelE tnecrep yb ssam
= noitartnecnoc ni lm/gr x 0.01
Recommended flume, ,enelyteca-ria gnizidixo ssam ni g fo elpmas
( ,nael eulb .)
5.7 Determination of Ziuc
5.5 Sample Preparation
tnuoM cniz wolloh edohtac lamp, tes -evaw
55.1 ekaT 10 g fo elpmas and refsnart ot .rekaeb htgnel at 9’312 mn and esimitpo eht tnemurtsni
Add 35 lm fo cirolhcordyh dica and 10 lm fo as rep snoitcurtsni manual. etingI eht .emalf
etulid cirtin dica ( 1 : 1 .) nehW noitulossid is etaripsA dellitsid retaw and adjust eht -rosba
,etelpmoc liob nwod eht yassa ot a ypurys ecnab ot .orez droceR eht secnabrosba fo
.ycnetsisnoc refsnarT eht stnetnoc ot 100 lm snoitulos A, B and C.
cirtemulov ,ksalf ekam up ot emulov and xim
.ylhguoroht
5.7.1 Calculation
5.5.2 ettepiP tuo 20 lm hcae fo eht elpmas otni
,cniZ tnecrep yb mass = 002)~u)~Q’b(z;(
owt 100 lm standard .sksalf Mark meht as B
and C. ekaM up B htiw etulid cirtin dica
( 1 tnecrep .) oT C add 1 lm hcae fo standard
erehw a2 b, and 2c era secnabrosba fo -ulos
,reppoc ,cniz dael and nori noitulos ( 100 mpp )
snoit A, B and C .ylevitcepser
and ekam up htiw etulid cirtin dica ( 1 tnecrep .)
5.8 Determination of Lead
5.5.3 Blanlz Solution
tnuoM eht dael wolloh edohtac lamp, tes -evaw
eraperP a tnegaer blank gniniatnoc eht emas
htgnel at 0’712 mn and esimitpo eht tnemurtsni
tnuoma fo stnegaer and yllacihpargortceps erup
as rep eht snoitcurtsni manual. etingI eht .emalf
muimdac latem daetsni fo elpmas and nekat
etaripsA dellitsid retaw and adjust eht ecnabrosba
hguorht 5.5.1 and 5.9.2. Mark eht blank
ot .orez droceR eht secnabrosba fo snoitulos A,
noitulos
as A. B and C.

5.6 Determination of Copper 5.8.1 Calculation
ngilA eht .tnemurtsni tnuoM reppoc wolloh
( b, - a~ )
edohtac lamp, tes htgnelevaw at 8’423 ,mn slit ,daeL tnecrep yb mass =
htdiw at 7’0 ,mn deef lamp tnerruc and esimitpo ( 3c - bs ) X 200
eht tnemurtsni as rep eht snoitcurtsni manual. erehw a3, b3, and 3c era secnabrosba fo -ulos
nruT no ,ria enelyteca and .emalf etaripsA snoit A, B and C .ylevitcepser
dellitsid retaw and adjust rof orez .ecnabrosba
nehT etaripsa standard reppoc noitulos ( 5 )mpp
5.9 Determination of Iron
and adjust eht tnemurtsni ot esimixam -rosba
ecnab ( tuoba 53’0 ecnabrosba units .)
tnuoM eht nori wolloh edohtac lamp, tes -evaw
htgnel at 3’842 mn and esimitpo tnemurtsni as
etaripsA blank noitulos A and drocer rosba
rep eht snoitcurtsni manual. etingI eht .emalf
ecnab fi .yna oslA etaripsa elpmas noitulos B etaripsA dellitsid retaw and adjust eht ecnabrosba
and ( elpmas + standard ) noitulos C. droceR
ot .orez droceR eht secnabrosba fo snoitulos
ecnabrosba ni hcae .esac An egareva fo at tsael
A, B and C.
evif sgnidaer is nekat ni hcae esac ( eef etoN 2 .)
5.6.1 Calculation 5.9.1 Calculation
lb - a, ( b4 - ~4)
,reppoC tnecrep yb mass = ,daeL tnecrep yb mass =
( ~1 - lb ) x 200 ( 4c - 64 ) x 200
erehw a,, bI and lc era secnabrosba fo noitulos erehw ad, b4 and 4c era secnabrosba fo -ulos
A, B and C .ylevitcepser snoit A, B and C .ylevitcepser
IS 13963 ( Part 1 ) : 1994
6 DETERMINATION OF COPPER BY THE 6.3.4 Calibration Curve
SPECTROPHOTOMETRIC METHOD
ekaT 0, 1, 2, 3, 4 and 5 lm fo eht standard
reppoc noitulos ( 6.2.8 ) ni a seires fo 150 lm
6.1 Outline of the Method
.srekaeb Add 5 lm hcae fo enimalyxordyh
elpmaS is devlossid ni cirolhcordyh dica and edirolhcordyh and ciratrat dica and deecorp as
cirtin .dica reppoC tneserp is decuder ot eht ni 6.3.1 and 6.3.2. droceR eht ecnabrosba fo
suorpuc etats htiw enimalyxordyh ,edirolhcordyh standard snoitulos and draw eht noitarbilac
corn lp dexe htiw niorpucohtab tnegaer and .evruc
detamitse yllacirtemotohportceps at 457 .mn
6.3.5 Calculation
6.2 Reagents
,reppoC tnecrep yb mass = % x 100
6.2.1 Hydrochloric Acid, dr = 61’1 ( -mrofnoc
gni ot SI 265 : 1993 ) erehw
6.2.2 Nitric Acid, dr = 24’1 gnimrofnoc( ot A = mass ni ,gm fo reppoc tneserp ni
SI 264 : 1976 ) ;elpmas and
B = mass ni ,gm fo elpmas .nekat
6.2.3 Dilute Sulphuric Acid, 50 tnecrep ( v/v .)
6.2.4 Hydroxylamine Hydrochloride, 10 tnecrep 7 NOITANIMRETED FO IRON YB
( m/v) ni cirolhcordyh dica 1 M. CIRTEMOTOHPORTCEPS DOHTEM
7.1 eniltuO fo eht dohteM
6.2.5 Tartaric Acid, 10 tnecrep ( m/v ) ni .retaw
elpmaS is thguorb otni noitulos htiw etulid cirtin
6.2.6 Bathocuproin Reagent, 0’02 .tnecrep .dica cirtiN dica is neht devomer vb baking
htiw cirolhcordyh dica and eht mass’ is nekat IC
evlossiD 0’2 g fo niorpucohtab ni 1 ertil fo iso otni noitulos ni cirolhcordyh .dica Cadmium is
lyma .lohocla devomer yb negordyh .edihplus retfA lavomer fo
negordyh ,edihplus nori is decuder ot tnelavid
6.2.7 Ammonia Sohition, 5 tnecrep ( V/V .) etats yb eht noitidda fo enimalyxordyh -ordyh
.edirolhc ehT ruoloc is neht depoleved yb eht
6.2.8 Standard Copper Solution ( 1 ml = 5 Pg noitidda fo~ 1 : 10 enilorhtnanehp and eht
uc ) ecnabrosba fo eht noitulos derusaem at 510 .mn
ekaT 1’0 g fo erup reppoc ( ytirup 99’99 tnecrep 7.2 stnegaeR
nim )~and evlossid ni 5 lm fo etulid cirtin dica
( 1 : i .) lioB eht noituloS and refsnart ot 1 ertil 7.2.1 Hydrochloric Acid, rd = 1.16,( conforming
cirtemulov .ksalf ekaM up ot eht .kram sihT ot SI 265 : 1993 .)
noitulos sniatnoc 100 pg fo reppoc rep .lm
etuliD 5 lm fo this noitulos ot 100 .lm ehT lanif
noitulos sniatnoc 5 pg fo reppoc rep .lm 7.2.2 Nitric Acid, dr = 24’1 ( gnimrofnoc ot
SI 264 : 1976 .)
6.3 Procedure
7.2.3 Hydroxylamine Hydrochloride Solution.
6.3.1 ekaT 5 lm fo eht elpmas noitulos deraperp 100 =til/g _
rednu 5.5 ni 150 lm .rekaerb Add 5 lm hcae fo
enimalyxordyb edirolhcordyh and ciratrat dica evlossiD 10 g fo enimalyxordyh edirolhcordyh
snoitulos and ekat eht yassa ot .liob looC and ( lCH.&NOH ) ni tuoba 60 lm fo retaw and
adjust eht Hp ot tuoba 5.5 yb noitidda fo etulid etulid ot 100 .lm
ainomma noitulos ( 5 tnecrep .)
7.2.4 Standard Iron Solution ( 1 lm = 10’0 gm .)
6.3.2 refsnarT ot 150 lm gnitarapes .lennuf Add evlossiD 001’0 0 g nori~fo 10 lm cirolhcordyh
of
20 lm niorpucohtab .tnegaer ekahS llew rof eno dica ( 1 : I ) and I lm fo enimorb .retaw lioB
.etunim wollA sreyal ot .etarapes niarD ffo litnu ssecxe enimorb is .devomer Add 200 lm
eht suoeuqa reyal and daer eht ecnabrosba fo fo cirolhcordyh ,dica looc and etulid ot 1 .ertil
eht tnegaer reyal ni a retemotohportceps at 457 etuliD 100 lm fo this noitulos ot 1 .ertil
.mn A blank nekat hguorht all eht stages fo
eht erudecorp is desu as a ecnerefer .noitulos
7.2.5 Ortho Phenanthroline Solution ( 3 l/g )
6.3.3 trevnoC ecnabrosba gnidaer fo eht elpmas
noitulos ot gm fo reppoc morf eht noitarbilac evlossiD 9’0 g fo enilorhtnanehp-o ni 30 lm fo
dna-lonahtem etulid ot 300 lm htiw .retaw
evruc and etaluclac eht egatnecrep fo .reppoc

3
3s 13963 ( traP 1 ) : 1994
.dilos dica ot evomer negordyh edihplus morf eht
7.2.6 Iron Sulplzide,
noitulos ( ees etoN 3 .) nehW negordyh edihplus
7.3 Calibration Curve is ;devomer etulid eht noitulos ot 80 .lm Add
5 lm enimalyxordyh ,edirolhcordyh 5 lm tnegaer
refsnarT. 0 ( tnegaer blank ) 2, 4, 6, 8 and 10 lm and adjust eht ph morf 3 ot 4 yb adding
ylevitcepser fo standard nori noitulos ot hcae fo muinomma edixordyh ro etulid cirolhcordyh
xis 100 lm cirtemulov .skssif etuliD ot 80 lm .dica Wait rof 15 setunim ot ezilibats eht ruoloc
htiw. dellitsid .retaw Add 5 lm fo enimalyxordyh and erusaem eht ecnabrosba at 510 mn against
edirolhcordyh ,noitulos ekahs and neht add 5 lm tnegaer blank ni retemotohportceps using 1 mc
fo tnegaer .e.i 1 : 10 enilorhtnanehp noitulos ot .llec trevnoC eht ecnabrosba gnidaer ot pg fo
poleved, ( der ruoloc .) retfA 15 etunim drocer nori morf eht noitarbilac :.vruc and etaluclac eht
eht ecnabrosba fo hcae noitulos at 516 .mn egatnecrep fo .nori
Draw eht noitarbilac evruc yb gnittolp -orcim
NOTE 3 - nI esac nori noitartnecnoc ni eht
grams fo nori as noitcnuf fo .ecnabrosba
elpmas si ,erom take elbatius touqila dna .deecorp
7.4 Procedure 7.5 Calculation
ekaT‘ 1 g fo eht .elpmas evlossiD ni 10 lm fo
,norI tnecrep yb mass = m :f BoI
etulid cirtin dica ( 1 : 1 .) retfA eht latem is
thguorb otni ,noitulos add cirolhcordyh dica
and etaropave ot .etsap Again add 10 lm erehw
cirolhcordyh .dica lioB and etulid ot 100 .lm
= mass ni pg, fo eht nori ni eht ;elpmas
Pass negordyh edihplus gas ot evomer muimdac M
and
( wolley .)etatipicerp retliF ffo eht etatipicerp
and liob eht noitulos htiw 20 lm cirolhcordyh mass ni g, fo eht elpmas .nekat
m =