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(Reaffirmed 2013) 
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(Reaffirmed 2012) 

(Reaffirmed
  2018)

(Reaffirmed 2011) 

(Reaffirmed 2010) 

(Reaffirmed 2009) 
h&an Standard  
METHOD FOR EMISSION SPECTROMETRIC
(Reaffirmed 2008) 
ANALYSIS OF PLAIN CARBON AND LOW
 
ALLOY STEELS POINT TO PLANE TECHNIQUE
(Reaffirmed 2007) 
( First Revision )
 

(Reaffirmed 2006) 
ICS 77.080.20
 

(Reaffirmed 2005) 

BUREAU OF INDIAN STANDARDS


MANAK BHAVAN, 9 RAHADUR SHAH ZAFAR MARC;
NEW DELHI I 10002

Price Group 3
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Mc~lrc~ls 01’ Chemical Analysis 01‘ Ferrous Metals Sectional C’ommi~(cc, MT11 2

I’his Indian Standard (First Revision) was adoptedby the Bureau of Indian Standards, after the tl~.at’t t‘inali/ctl
hy fhc Mcthocls of‘ Chemical Analysis of’ Ferrous Metals Sectional Commitbz had hccn apt~ovccl by llrc
Mctallur~ical Engineering Division Council.

This slantlard has hccn prepared with ;I view to incorporate the latest dcvclopments in Ihc I’icltl 01 cmissioli
spcclroniclric analysis.

‘l‘hiss~ancl~~rtlwas lirst hi-ough; out in 1978. The first revision has hccn undcrtakcn 10 take inlo ac~x~unt
the cxpcriencc gait& during the period. The method dcscribctl in this standard is rccommcndccl I‘or.analysi\
(11.plain carhon and low alloy steels samples of’ suitable shape and size for all clemen~s I‘oI. which IIIICS
arc availahlc in the cnlission/v~lcuurn emission spcctromctcr by point to plane spark ~cchnictuc.

‘l‘lic mclallurgic;il state of ccl-lain alloys may have some influence on the spectral emission. In lhcsc ins(ances.
s;miplcs and rclixcncc nialerials shall be in the same mclallurgical slate.

I+v tlic p~irposc 01‘ dccidin g whcthcr a particular- rcquircmenl of‘ this standai-d is compticd wilh, lhc 1’1n;rl
\~;iluc. clt~scrved or calculated, cxprcssing the ircsult of’ a lest 01. analysis, shall he I-ouridcd ol‘l‘ in ;~ccordiincc
wirh IS 2 : I960 ‘Rules for rounding oft‘ numerical values (rc~~i.scrl)‘. The iiu~i~lxi~ of‘ signific;\nl pl;icc~
rc‘~;~~nctl 111 ~IIC ~rountlcclol‘l‘ value should he snmc as that 111‘lhc spccil‘icd value in this sl;mtlartl.
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IS 8811 : 1998

Indian Standard
METHOD FOR EMISSION SPECTROMETRIC
ANALYSIS OF PLAIN CARBON AND LOW
ALLOY STEELS POINT TO PLANE TECHNIQUE
( First Revision )
1 SCOPE impurity in plain carbon and low alloy steels with
a minimum iron content of 94 pa-cent. The possible
1.1 This standard gives a generalised spectrometric analytical and internal standard lines alongwith the
analysis procedure for determining the following concentration ranges are also given below I’OI
clcments when present as alloying element or as . information:

Analytical Line Internal Stamhd Line Concmtrution Range


(nm) (nm) (pa-cent by mass)

Aluminium 394.4 27 I .44 0.005 lo 0. IS


308.2

At-senic 197.20 27 1.44 0.005 to 0.05


193.76

Boron 182.64 27 I .44 0.005 to 0.010


I X2.59

Carbon 193.09 27 1.44 0.01 to I .s

Chromium 29X.92 27 1.44 0.05 to 5.0


267.72 27 1.44

Cobalt 345.35 27 I .44 0.01 to 0.20


22X.62

Copper 327.40 2.7 I .44 0.01 to 0.5


213.6

Manganese 293.3 I 27 I .44 0.01 to 2.0


255.86

Molybdenum 379.83 27 I .44 O.OI to I.5


277.54
3X6.4 I

Nickel 288. I6 27 I .44 0.05 to 5.0


7CI L1
LJ I.111

Niobium 3 I Y.5 27 I .44 0.008 to 0.076

Phosphorus 17X.29 271 44 0.005 to 0. IO

Silicon 28X.16 27 I .44 0.05 to 2.0


51.61

Sulphul 1X0.73 27 I .44 0.005 to 0. IO

Ti 11 I XY.YY 271 44 0.003 lo 0. IO

‘I‘itaniuni 337.28 271 44 O.O! lo 0.25

Vanadium 3 10.23 27 I .34 0.01 to I .o


3 I I .07

Zirconium 343.X2 27 I .44 0.00 I to 0.05

I
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IS 8811 : 1998
1.2 Marc clcments and varied detection limits can 4.7 If’ the spectrometer is provided with VXLIUI~
he achicvcd hy choosing suitable lines while selecting system, it shall be the manufacturer’s choice.
the spcctromcter.
NOTES

2 REFERENCE

2.1 ‘lk following Indian Standard is a necessary


aci.jLinct to this standard:

IS No. Title
7072: 1971 Glossa~-y of‘ terms relating to
emission spectroscopy

3 SIJMMARY OF METHOD
5 ELECTRODES
3.1 The sample is excited by controlled spark/
clisc:hargc. Lisiny a point (counter clcctrode) to plane 5.1 The counter electrode shall hc of pure silver or
(polished l‘lat surl.>lcc of sample). The radiation from thoriated tungsten.
sl~;Lrk/~li~ch~trfe. is dispersed hy a quartz prism/grating.
‘l’hc radiant cricrgy (intensity) ol‘the selected analylical 5.2 The shape and angle of upper tip shall he ;IS pc~
lines arc convci-ted lo electrical impulses by the requirement of the instrument.
piiotonLiiltil~licr tLlhc, which is amplified and stored
in capacitor. ‘I’hc charge from cuch capacitor is 5.3 The clectrodc :uncl tip shall hc kept clean.
nle;ibLlrccl and converted into intensity ratios. ‘l‘hC
~c~l~c~lltl’ilti0ns 01‘ elelll~llts arc calculated f.rom 5.4 ‘l‘hc spark gap hctwccn clcctrodc and specimen
analytical working cLIrvcs pi-cparcd hy exposing shall hc as per the manuf’acturcr’s instruction manual.
slantlard samples of’ similar type.
6 SPARK STAND AND ARGON SYSTEM
4 SPECTROMETER AND GENERAL
REQUIREMENTS 6.1 Spark stand shall hc mounted directly on the
spectrometer, and equipped to hold flat specimens
4.1 Any make ol‘spcctrometcr having good reciprocal and counter electrode.
linear dispersion and good resolution is rccommcnded.
‘I’hc sensitive lines of certain elements like carbon, 6.2 Argon flow connection dul-in: flushing and
sulphur. phosphorus, arsenic, horon, etc. are in vacuum sparking with automatic controls shall he provided
LIIII.;I violet region. To avoid ahsorption of radiation on the spark stand.
of‘ thcso lines. ;I vacuLim type spcctromctcr is mosl
slllt;lhlc~.

4.2 ‘I‘lw spcctromcter sl~ould have ;I wave length 6.4 Argon shll hc ollpuiity W.W5 percent minimum.
~~)vcr;Lgc (,I’ I 700 to 4 OOOA” I‘or analytical lines. A rcclucing atmospheric l’urnacc at 425/450” C with
My/I‘i molecular sicvcs shall hc used to I-CIIIOVC
4.3 Focal length, grntins parameters, reciprocal linear oxygcn/moistLirc tracts l‘rom argon.
tliapcl-sion, primary slit width, secondary slit width
antI W;IVC Icnyth covcragc shall he as per
uianL~f:ictLIrer-‘s discretion.

4.4 ‘l‘hc lines selected for each elcmcnl shall bc 01 6.5Argon pressure and I~low rate shall he ;I’; pa
pr~~vcn satisfactory rcproducihility. Though, Illost of‘ manul;Lcturei-‘s iiiX;tl-uclion.
~hc lines arc COII~IUOI~, the lines shall hc s~le~tcd by
the Illstruwcnt manLiI‘;icturcr to get maximLLm optical 7 EXCITATION SOUR<‘E
output with minimLull intci-lcrenuc.

4.5 ‘l‘hc \pcctromctcr shall hc kept in the following


I;lhol-atory cllvil-onmcnts:

‘l‘clllpel-atlll-c 19°C to 25°C‘ 7.2 ‘I’hc excitation pal-amctcrs dcpcnd IIEI~III~ (III tl~c
liclnti\,c llunlitlity ‘15 to 60 pcrccnl nature 01‘ sallq~lcs to bc ;lI1;Lly\,'cI,c'lclllcIlls antI the
Atlllosphcrc I)ust-II-CC ccniccntr;ltion levels to lit dctcrminatcd. These: can
hc xllicvcd by dil’icl-cnt combinations 01 capacitance.
4.6 clccti.ic powc‘r tolcrancc shall he + 5 pcrccnl
‘I‘hc pol~i~rial (voltage). Ircbi5l;rncc and intluctancc. Each
lxcluahly _t 2 pcr~cnr and I’iltcl-cd to ~~rcvcnl IradIo manul’acturcr rccommc’nds special conltlln;ltic)iis.
i’~c’qucncy intcrl‘ci-cncc. Lvith good i-.1’. grc~undin~ Hc~wcvcl-, ~01IIcc p;r;llllelcl-s used sllcccssl‘Lllly hy
syhtcm when worhiny with nlicroproccssor!- ad ~!\cr;iI lahoi~;tlorics arc :_ri\,cri in Annex I3 :~nd C;III
I‘oIIlpLItcl~s.
IX used ;IS ~Liid:uicc.
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IS 8811 : 1998
7.3 ‘l‘hc SOUI-cc paramclcra shall also include peak 10 STANDARD SAMPLES
current, current pulse dulntion and number 01’
dischqcs per second. 10.1 Standxd smplcs shall hc of two types:

a) Pri/lrclr-J Srcllltlrl~r/.s - prI’eI‘crahly frolll


7.4 The established parameters sl10~11d bc available
qualil‘ied agencies engaged in preparation 01‘
with each spcc~mnetcr.
spectrographic standards.

7.5 Pre-burn period, cxposurc period and exposure b) bVo~&q Strduds - Thcsc are PI-cparcd by
conditions shall be esk~blishcd by the user depending the LISC~ depending upon his product range
upon the type of samples heing analysed and as per and type 01‘ composition.
IIICI-ccommendations of‘ the manufacturer. However,
the pw~mctcrs given in Annex C wcrc: sucessfully 11 CALIBRATION AND STANDARDIZATION
usctl in SCVCI-al lahol-atorics and thus can he used as
~~tiitlancc. 11.1 The spectrometer shall hc slnbilised as per the
manufacturer’s instruction, and alI lhc paramelcrs
8 MFXSIJRING SYS’IWM regarding profiling, vacuuni, ai-gon Ilow, excitation
conditions arc set to the rccluircd Icvcl.
X.1 'I‘hc spccti-OIIIC~CI- nicasurin g systcni consists 01‘
I~lic~t~)-~~iullil,Iicr luhcs wilh individual voltage Il.2 The internal standard rnethocl shall hc qq~licd
;ltl,jtl>tlllcnts, ;mlpliI‘icI-s. capacitors
to store the oL~t- I‘or mcasurins lhc intcnsily or radiant cncrgy 01‘
put volta~c ;111(1 sys~cn~ to IIIWSLIW
the capacitor dilt‘crcnt lines and f)r making working curves. In
cl~argcs and ~~i-~~yr;iinmcs I‘or tlic sequence 01‘ thih incthod, the discharge is ~erniinatetl a( ;I
cqwaticma.
prctlctc~-niinctl accuniulalccl lcvcl 01’ inlcnsity 1‘01
intci-nal stnndard iron line.
8.2 Ieor rnca5liriny lhc capacitor charge, dil.fct-cnt
\)‘SlClll!3 Llsi‘d
ill-C ;~ncI shall hc as per the 11.3 Using low and high alloy coniposition st~indards
i.I’c~oi~Iii1cIi(I;itioils 01‘ tlic ni~inui’r~cturcr. set the dynodc/~lttcnu~ltcl- to control the photomultil~licl
tLihc, to get the reqLiirctJ voltage output I’or each line
Ihr miniiiitmi and mixiniufn perccnlagc ol‘thc clcnicnl.
9 SAMPLING; AND SAMPLE PREPARATION
11.4 Excite standard s~~~mplcs with vai-yin: clcnicnl;il
0.1 S;llnplc l‘or sp,cctl~olllctcl~ analysis shall 1x2 01‘
perccnt:ipcs SCVCI-aI tirncs (to take C;II-c 01‘ lhc shoi-t
a~q~~ox~~~~at~ 30 to 40 tnli~ tliamclcr alId IO to 20
term drift) and iiic;isL~i~c the inlcnsity
nim thickness. Sninllci~ si/c is not rccomnicndcd
due to hcatiny 1113 clut-ing cxcilation and spark
11.5 The working curve shall hc prcp;lretl as in 11.2,
drschN~c.
vising intciis~ty ratios 1.3 concciitr;ilic~n ratios.

0.2 Salllplc pl CKlLlCCCl shall IX Ilolllo~t‘ncoLls and free


11.6 Dcpcndin~ upon the Liscr pro~raninic. widci
l‘roni porosity. voids and inclusions.
conccnti-alion r~un~cs can hc plotted in scgmcnts with
expanded scdes.
9._3 All)' 01' the I’~lllowin, I’ lll~lhocls shall hc LISaI l.or
liquid steel sampling:
11.7 While preparing curves the I‘ollowin~ points Iiavc
to hc taken into account:
I’oul-ins into i.a<l-iron nloultl,

I’ouriiig into coppci- 1110~ilcls (single or split a) Background correction,


lyl’“). ;111d
h) Inter-clemcntal intcrl’crcncc.
c) Metallurgical conditiori/st~ltc. and

cl) Analytical CIII-vc shil’t/rotatitrn.

In most 01‘ the latc5t \,cl-sion 01‘ qdronictcrs, Ihc


sol‘tw;~rc suppliccl by the riranLll’acturci~ c~~lc~~latcs lhe
coi-rcction Ior the aho\~c l~;ictors. ‘l‘licsc arc’ cxpl~iinctl
hriltily in 1 1.7.1 to 1 1.7.4,

11.7.1 l~lll~-tl~-l~a~l~~l~oLlll~~ col‘l'eclic,ll l1as to I,?


;lppllL!d IOI. CXIl cllallllcl/llllc ((1 ycL ;lccLllatc IllOIL!

;rn;ilysis. Icvcl~. ‘i‘liis


c5p~*‘,iall\, in lti\\~~~i~~~oii~~~~iI~;tIioii
IS 11~)1111;111\
dOllC I>\. \ul~tl~aCllll~ lllli’ I~;I~I\?Il-oIIIliI
i~exlinp l‘roin the x.lti;il intensity oulpLil. ‘1‘11~ ~li.lcct~on
llllllt I\ ;11<1 ~I1IIJI1c~c’II I’\. ‘I) ll;lllllL’ I~;l~~h~~l-c~lllltl
col-I~CllOll.

11.7.2 In nlany C;ISCS. intcrlcrcllics lroiii otlicr


clclllellls arc sr~n~lic;~nl. c\pcci:lIly ;~t l0wc.i.
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IS XXII : 1998

~~)nccnlralion Icvcls. This may Icad LOsuppression 12 PROCEDURE


01’ enhancement of intensity. Interf’erence factor is
c~~~thlished hy exposing different standards of varying 12.1 Set-up the spcctometcr as pcl- the standard
Iiialrix composition. procedure, clean the excitation stand and elcctrodc.

11.7.3 Corrections for metallurgical state/condition 12.2 Prepare the sample as pei- 9.
arc applied as per users choice of samples. This is
nol-mally achicvcd by selection of working standards
12.3 Excite the sample and take intensity readings
01‘ \inlilar mctalluryicnl condition as that of samples in duplicate or triplicate.
IO hc analyscd. The working curve prepared from
primary standard a~-e corrected by exposing the
12.4 From the average intensity reading calculate the
working stardar-ds. These are also known as type
concentration of different elements from the working
4l~~iitl~~r~liz~~tio~i.
curve.
Il.74 Analytical curve sliil‘t/i-ot~ition is caused by
ll~ dii-ly optics, change in optics, excitation source, 12.5 Conversion of scale, digital voltmctcr or pi-int-
lint vol(;tgc, spcctromctc~- clectrnnics and ambient out readings into element percentages, coupled with
room cc~ntfi~io~~s. Excite a set of standards, and taken evaluation ol’ correction factors, may also bc carried
inlcnsify readings and correct the curves for drift. out through computers and programmable calculators,
which al-e pi-cviously progrimimcd with correction
11.X Accuracy 01‘ standardization dcpznds mainly on and calibration data. Each curve is stored in memory.
lhc long-term stability of’ the emission spectrometer. A linear arithetic I’oI-mula or polynomials of second
II the values XC: within the standard dcvintions of OI- higher ordcl-s have ken used to represent analytical
the s~andxtl m~nplcs, no correction need be applied. curves in the memory register of the automatic devices.
II thcrc IS considcrahly deviation, recalibrate and Conversion of intensily ralio into concentmtior~ is
rccstahlish the curve. done autoinaticnlly.

11.9 The instrument and calibration shall be evaluated 12.6 Latest model spectrometers are equipped with
pcriotllcally and standard errors nre corrected, so as visual display units and printouts for obtaining
lo cnahlc llic opcralor to get accurate results. results.

ANNEX A
(Cluuse 4.7, Note)
INSTRUMENT PARAMETERS
Focal Icngth 0.75 to I .o Ill

Wave Icngth covcragc I 700 lo 4 000 A”

licciprocal lineai
dispersion 6 A” mm Mill
VacuLlm 2.5 pm or hclow

Primary slit width 33 PI11 to .50 pm

Secondary slil width 30 pii to 200 pin

ANNEX B
(Cl~rusc7.2)
SOIJRCE PARAMETER8
Capacitance, pF IO to IS
Inductance, I.IH so (0 70
Kcsixtancc 3 lo 5
r~otcnti~li.
v 940 to I 000
I. I. clll~l~enl. A 0.3 to 0.x

I )Iscll;ll-gC/scC ho

()ncc paramelcrh (sclcctecl I’I-oin Ihis) :11-c chUt3llshctl. iii;iintaiii them cal-ct‘iilly.

3
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IS xx11 : IWX

ANNEX C
(Clrr11.w 7.5)
EXPOSURE CONDITIONS

5 to IS see

5 10 20 see

3 to 30 see

2.5 to 25 I/ iiiiti

2.5 to 25 I / min

25 lo I.5 Ilrnin

90” to I20”

3 to 5 111111
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harmonious development of the activities of standardization, marking and quality certification of goods and
attending to connected matters in the country.

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implementing the standard, of necessary details, such as symbols and sizes, type OI pde designations.
Enquiries relating to copyright be addressed to the Director (Publications), BIS.

Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed
periodically; a standard along with amendments is reaffirmed when such review indicates that no changes
are needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian
Standards should ascertain that they are in possession of the latest amendments or edition by referring to
the latest issue of ‘BIS Handbook’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Dot : MTD 2 (3662).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

BUREAU OF INDIAN ST,%NDARDS

tlcxlcpa7Iel-s :

Manal; Bhavan, 9 Bahadur Shah ‘&far Marg, New Delhi- I IO002 Tclegratns : Manaks~~na~l~a
‘l’clcl~llollcs : 323 01 3 I. 323 33 75, 323 94 02 (Co~ii~iio~i to aI1 ol’l‘iccs)

Kcgional 0l‘l‘icc.s : ‘I’clcphonc

Cclltrnl : Manak Bhavan, 9 Bahndur Shah Zafar Marg Jm 7~117


NEW DELHI I 10002 1321 3s4 I

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