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IS 8811 (1998): Method for Emission Spectrometric Analysis
of Plain Carbon and Low Alloy Steels Point to Plane
Technique [MTD 16: Alloy Steels and Forgings]
h&an Standard
METHOD FOR EMISSION SPECTROMETRIC
ANALYSIS OF PLAIN CARBON AND LOW
ALLOY STEELS POINT TO PLANE TECHNIQUE
( First Revision )
ICS 77.080.20
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 RAHADUR SHAH ZAFAR MARC;
NEW DELHI I 10002
Price Group 3






Mc~lrc~ls 01 Chemical Analysis 01 Ferrous Metals Sectional Commi~(cc, MT11 2
Ihis Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the tl~.att tinali/ 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 Iicltl 01 cmissioli
spcclroniclric analysis.
lhis s~ancl~~rtl was 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 Ior.analysi\
(11. plain carhon and low alloy steels samples of suitable shape and size for all clemen~s IoI. which IIIICS
arc availahlc in the cnlission/v~lcuurn emission spcctromctcr by point to plane spark ~cchnictuc.
llic 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 11n;rl
\~;iluc. clt~scrved or calculated, cxprcssing the ircsult of a lest 01. analysis, shall he I-ouridcd oll 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 ~rountlccl oll value should he snmc as that 111 lhc spccilicd value in this sl;mtlartl.





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 IOI
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
Iitaniuni 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




IS 8811 : 1998
1.2 Marc clcments and varied detection limits can
he achicvcd hy choosing suitable lines while selecting
the spcctromcter.
2 REFERENCE
2.1 lk following Indian Standard is a necessary
aci.jLinct to this standard:
IS No.
7072: 1971
Title
Glossa~-y of terms relating to
emission spectroscopy
3 SIJMMARY OF METHOD
3.1 The sample is excited by controlled spark/
clisc:hargc. Lisiny a point (counter clcctrode) to plane
(polished llat surl.>lcc of sample). The radiation from
sl~;Lrk/ ~li~ch~trfe. is dispersed hy a quartz prism/ grating.
lhc radiant cricrgy (intensity) olthe selected analylical
lines arc convci-ted lo electrical impulses by
piiotonLiiltil~licr tLlhc, which is amplified and stored
in capacitor. Ihc charge from cuch capacitor is
nle;ibLlrccl and converted into intensity ratios. lhC
~c~l~c~lltlilti0ns 01 elelll~llts arc calculated f.rom
analytical working cLIrvcs pi-cparcd hy exposing
slantlard samples of similar type.
4 SPECTROMETER AND GENERAL
REQUIREMENTS
4.1 Any make olspcctrometcr having good reciprocal
linear dispersion and good resolution is rccommcnded.
Ihc sensitive lines of certain elements like carbon,
sulphur. phosphorus, arsenic, horon, etc. are in vacuum
LIIII.;I violet region. To avoid ahsorption of radiation
of thcso lines. ;I vacuLim type spcctromctcr is mosl
slllt;lhlc~.
4.2 Ilw spcctromcter sl~ould have ;I wave length
~~)vcr;Lgc (,I I 700 to 4 OOOA Ior analytical lines.
4.3 Focal length, grntins parameters, reciprocal linear
tliapcl-sion, primary slit width, secondary slit width
antI W;IVC Icnyth covcragc shall he as per
uianL~f:ictLIrer-s discretion.
4.4 lhc lines selected for each elcmcnl shall bc 01
pr~~vcn satisfactory rcproducihility. Though, Illost of
~hc lines arc COII~IUOI~, the lines shall hc s~le~tcd by
the Illstruwcnt manLiI;icturcr to get maximLLm optical
output with minimLull intci-lcrenuc.
4.5 lhc \ pcctromctcr shall hc kept in the following
I;lhol-atory cllvil-onmcnts:
lclllpel-atlll-c 19C to 25C
liclnti\ ,c llunlitlity 15 to 60 pcrccnl
Atlllosphcrc I)ust-II-CC
4.6 Ihc clccti.ic powcr tolcrancc shall he + 5 pcrccnl
lxcluahly _t 2 pcr~cnr and Iiltcl-cd to ~~rcvcnl IradIo
i~cqucncy intcrlci-cncc. Lvith good i-.1. grc~undin~
syhtcm when worhiny with nlicroproccssor!- ad
I oI I l pLI t cl ~s.
4.7 If the spectrometer is provided with VXLIUI~
system, it shall be the manufacturers choice.
NOTES
5 ELECTRODES
5.1 The counter electrode shall hc of pure silver or
thoriated tungsten.
5.2 The shape and angle of upper tip shall he ;IS pc~
the requirement of the instrument.
5.3 The clectrodc :uncl tip shall hc kept clean.
5.4 lhc spark gap hctwccn clcctrodc and specimen
shall hc as per the manufacturcrs instruction manual.
6 SPARK STAND AND ARGON SYSTEM
6.1 Spark stand shall hc mounted directly on the
spectrometer, and equipped to hold flat specimens
and counter electrode.
6.2 Argon flow connection dul-in: flushing and
sparking with automatic controls shall he provided
on the spark stand.
6.4 Argon shll hc ollpuiity W.W5 percent minimum.
A rcclucing atmospheric lurnacc at 425/450 C with
My/ Ii molecular sicvcs shall hc used to I-CIIIOVC
oxygcn/ moistLirc tracts lrom argon.
6.5 Argon pressure and I~low rate shall he ;I; pa
manul;Lcturei-s iiiX;tl-uclion.
7 EXCITATION SOUR<E
7.2 Ihc excitation pal-amctcrs dcpcnd IIEI~III~ (III tl~c
nature 01 sal l q~l cs t o bc ; l I 1; Ll y\ , ' cI , c' l cl l l cI l l s ant I t he
ccniccntr;ltion levels to lit dctcrminatcd. These: can
hc xllicvcd by dilicl-cnt combinations 01 capacitance.
pol~i~rial (voltage). Ircbi5l;rncc and intluctancc. Each
manulacturcr rccommcnds special conltlln;ltic)iis.
Hc~wcvcl-, ~01IIcc p;r;llllelcl-s used sllcccsslLllly hy
~!\ cr;iI lahoi~;tlorics arc :_ri\ ,cri in Annex I3 :~nd C;III
IX used ;IS ~Liid:uicc.





7.3 lhc SOUI-cc paramclcra shall also include peak
current, current pulse dulntion and number 01
dischqcs per second.
7.4 The established parameters sl 10~11d bc available
with each spcc~mnetcr.
7.5 Pre-burn period, cxposurc period and exposure
conditions shall be esk~blishcd by the user depending
upon the type of samples heing analysed and as per
IIIC I-ccommendations of the manufacturer. However,
the pw~mctcrs given in Annex
usctl in SCVCI-al lahol-atorics and
~~tiitlancc.
8 MFXSIJRING SYSIWM
C wcrc: sucessf ul l y
thus can he used as
X. 1 ' I hc spccti - OI I I C~CI - nicasurin g systcni consists 01
I~lic~t~)-~~iullil,Iicr luhcs wilh individual voltage
;ltl,jtl>tlllcnts, ;mlpliIicI-s. capacitors to store the oL~t-
put volta~c ;111(1 sys~cn~ to IIIWSLIW the capacitor
cl~argcs and ~~i-~~yr;iinmcs Ior tlic sequence 01
cqwati cma.
8. 2 Ieor rnca5liriny lhc capacitor charge, dil.fct-cnt
\)SlClll!3 ill-C Llsid ;~ncI shall hc as per the
i.Ic~oi~Iii1cIi(I;itioils 01 tlic ni~inuir~cturcr.
9 SAMPLING; AND SAMPLE PREPARATION
0.1 S;llnplc lor sp,cctl~olllctcl~ analysis shall 1x2 01
a~q~~ox~~~~at~ 30 to 40 tnl i ~ tliamclcr alId IO to 20
nim thickness. Sninllci~ si/c is not rccomnicndcd
due to hcatiny 1113 clut-ing cxcilation and spark
drschN~c.
0.2 Salllplc pl CKlLlCCCl shall IX Ilolllo~tncoLls and free
lroni porosity. voids and inclusions.
9._3 Al l ) ' 01' the I~lllowin, I lll~lhocls shall hc LI SaI l.or
liquid steel sampling:
Ioul-ins into i.a<l-iron nloultl,
Iouriiig into coppci- 1110~ilcls (single or split
lyl). ;111d
IS 8811 : 1998
10 STANDARD SAMPLES
10.1 Standxd smplcs shall hc of two types:
a)
b)
Pri/lrclr-J Srcllltlrl~r/.s - prIeIcrahly f rol l l
qualilied agencies engaged in preparation 01
spectrographic standards.
bVo~&q Strduds - Thcsc are PI-cparcd by
the LI SC~ depending upon his product range
and type 01 composition.
11 CALIBRATION AND STANDARDIZATION
11.1 The spectrometer shall hc slnbilised as per the
manufacturers instruction, and alI lhc paramelcrs
regarding profiling, vacuuni, ai-gon Ilow, excitation
conditions arc set to the rccluircd Icvcl.
Il.2 The internal standard rnethocl shall hc qq~licd
Ior mcasurins lhc intcnsily or radiant cncrgy 01
diltcrcnt lines and f)r making working curves. In
thih incthod, the discharge is ~erniinatetl a( ;I
prctlctc~-niinctl accuniulalccl lcvcl 01 inlcnsity 101
intci-nal stnndard iron line.
11.3 Using low and high alloy coniposition st~indards
set the dynodc/~lttcnu~ltcl- to control the photomultil~licl
tLihc, to get the reqLiirctJ voltage output Ior each line
Ihr miniiiitmi and mixiniufn perccnlagc olthc clcnicnl.
11.4 Excite standard s~~~mplcs with vai-yin: clcnicnl;il
perccnt:ipcs SCVCI-aI ti rncs ( to take C; I I - c 01 lhc shoi-t
term drift) and iiic;isL~i~c the inlcnsity
11.5 The working curve shall hc prcp;lretl as in 11.2,
vising intciis~ty ratios 1.3 concciitr;ilic~n ratios.
11.6 Dcpcndin~ upon the Liscr pro~raninic. widci
conccnti-alion r~un~cs can hc plotted in scgmcnts with
expanded scdes.
11.7 While preparing curves the Iollowin~ points Iiavc
to hc taken into account:
a) Background correction,
h) Inter-clemcntal intcrlcrcncc.
c) Metallurgical conditiori/st~ltc. and
cl) Analytical CI I I - vc shilt/rotatitrn.
In most 01 the latc5t \,cl-sion 01 qdronictcrs, Ihc
soltw;~rc suppliccl by the riranLllacturci~ c~~lc~~latcs lhe
coi-rcction Ior the aho\~c l~;ictors. llicsc arc cxpl~iinctl
hriltily in 11.7.1 to 1 1.7.4,
11.7.1 l ~l l l ~- tl ~- l ~a~l ~~l ~oLl l l ~~ col l ' ecl i c, l l l1as to I,?
;lppllL!d IOI. CXI l cl l al l l l cl / l l l l c ( ( 1 ycL I l l OI L! ;lccLllatc
;rn;ilysis. c5p~*,iall\, in lti\ \ ~~~i~~~oii~~~~iI~;tIioii Icvcl~. iliis
IS 11~)1111;111\ dOllC I>\ . \ ul~tl~aCllll~ lllli I~;I~I\?Il-oIIIliI
i ~exl i np lroin the x. l ti ; i l intensity oulpLil. 111~ ~li.lcct~on
llllllt I\ ;11<1 ~I1IIJI1c~cII I\. I) ll;lllllL I~;l~~h~~l-c~lllltl
col - I ~Cl l Ol l .
11.7.2 In nlany C;ISCS. intcrlcrcllics lroiii otlicr
clclllellls arc sr~n~lic;~nl. c\pcci:lIly ;~t l0wc.i.





IS XXII : 1998
~~)nccnlralion Icvcls. This may Icad LO suppression
01 enhancement of intensity. Interference factor is
c~~~thlished hy exposing different standards of varying
Iiialrix composition.
11.7.3 Corrections for metallurgical state/condition
arc applied as per users choice of samples. This is
nol-mally achicvcd by selection of working standards
01 \inlilar mctalluryicnl condition as that of samples
IO hc analyscd. The working curve prepared from
primary standard a~-e corrected by exposing the
working stardar-ds. These are also known as type
4l~~iitl~~r~liz~~tio~i.
Il.74 Analytical curve sliilt/i-ot~ition is caused by
ll~ dii-ly optics, change in optics, excitation source,
lint vol(;tgc, spcctromctc~- clectrnnics and ambient
room cc~ntfi~io~~s. Excite a set of standards, and taken
inlcnsify readings and correct the curves for drift.
11.X Accuracy 01 standardization dcpznds mainly on
lhc long-term stability of the emission spectrometer.
II the values XC: within the standard dcvintions of
the s~andxtl m~nplcs, no correction need be applied.
II thcrc IS considcrahly deviation, recalibrate and
rccstahlish the curve.
11.9 The instrument and calibration shall be evaluated
pcriotllcally and standard errors nre corrected, so as
lo cnahlc llic opcralor to get accurate results.
12 PROCEDURE
12.1 Set-up the spcctometcr as pcl- the standard
procedure, clean the excitation stand and elcctrodc.
12.2 Prepare the sample as pei- 9.
12.3 Excite the sample and take intensity readings
in duplicate or triplicate.
12.4 From the average intensity reading calculate the
concentration of different elements from the working
curve.
12.5 Conversion of scale, digital voltmctcr or pi-int-
out readings into element percentages, coupled with
evaluation ol correction factors, may also bc carried
out through computers and programmable calculators,
which al-e pi-cviously progrimimcd with correction
and calibration data. Each curve is stored in memory.
A linear arithetic IoI-mula or polynomials of second
OI- higher ordcl-s have ken used to represent analytical
curves in the memory register of the automatic devices.
Conversion of intensily ralio into concentmtior~ is
done autoinaticnlly.
12.6 Latest model spectrometers are equipped with
visual display units and printouts for obtaining
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~rusc 7.2)
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 II-oin Ihis) :11-c chUt3llshctl. iii;iintaiii them cal-ctiilly.
3





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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This Indian Standard has been developed from Dot : MTD 2 (3662).
Amendments Issued Since Publication
Amend No. Date of Issue Text Affected
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