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Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to

information for citizens to secure access to information under the control of public authorities,in order to promote transparency and accountability in the working of every public authority,

and whereas the attached publication of the Bureau of Indian Standards is of particular interest

to the public, particularly disadvantaged communities and those engaged in the pursuit of

education and knowledge, the attached public safety standard is made available to promote the

timely dissemination of this information in an accurate manner to the public.

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Mc~rc~s

01

Chemical Analysis 01 Ferrous Metals Sec tional Commi~(cc, MT11 2

Ihis Indian Standard (First Revision) was adoptedby 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

Mc tallur~ca l 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~anc l~~rtlwas lirst hi-ough; out in 1978. The first revision has hccn undcrtakcn 10 take inlo ac~x~unt

the cxpc riencc gait& during the period. The method dc scribctl 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~cuurn 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

~IC ~rountlccloll value should he snmc as that 111hc spccilicd

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 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

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IS 8811 : 1998

1 2 Ma rc c lcments 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.

7 72: 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

clcc trode) to plane

(polished llat surl.>cc of sample). The rad iation from

sl~;Lrk/~i~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~icr tLlhc, which is amplified and stored

in capacitor.

Ihc charge from cuch ca pac itor is

nle;ibLlrccl and converted into intensity ratios.

lhC

~c~l~c~lltlil ti0ns 01 elelll~llts arc calculat ed f.rom

ana lytical working cLIrvcs pi-cpa rcd 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 vac uum

LIIII.;I violet region. To avoid ahsorption of radiation

of thcso lines. ;I vac uLim type spc ctromctcr is mosl

slllt;lhlc~.

4.2 Ilw spcctromcter

sl~oud

have ;I wave length

~~)vcr;Lgc (,I I 700 to 4 OOOA Ior analytical lines.

4.3

Focal length,

grntins parameters, reciprocal linear

tliapc l-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~e~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

lic lnti\ ,c llunlitlity

15 to 60 pc rccnl

Atlllosphcrc

I ust-II-CC

4.6 Ihc

clccti.ic powcr tolcrancc shall he + 5 pcrccnl

lxcluahly _t 2 pc r~cnr

and Iiltcl-cd to ~~rcvcnl IradIo

i~cquc ncy intcrlc i-cncc .

Lvith good i-.1. grc~undin~

syhtcm when worhiny with nlicroproccssor -

ad

I o I I l pL I t c l ~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 spa rk stand.

6.4 Argon

shll hc ollpuiity W.W5

percent minimum.

A rcclucing

atmospheric lurnac c at 425/450 C with

My/Ii molecular sicvcs shall hc used to

I-CIIIOVC

oxygcn/moistLirc trac ts lrom argon.

6.5

Argon pressure and I~ow rate shall he ;I; pa

manul;Lcturei-s iiiX;tl-uclion.

7 EXCITATION SOUR

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7.3 lhc SOUI-cc paramccra shal aso 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 sampes heing anaysed and as per

IIIC I-ccommendations of the manufacturer. However,

the pw~mct cr s

given in Annex

usctl in

SCVC-a

lahol-atorics and

~~tiitlancc.

8 MFXSIJRING SYSIWM

C

wcrc:

sucessfull 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 vota~c ;1111 sys~cn~ to IIIWSLW the capactor

cl~argcs and ~~i-~~yr;iinmcs Ior tlic

sequence 01

cqwati cma.

8.2

Ieor rnca5liriny lhc capacitor charge, dil.fct-cnt

\)SCll 3 ill-C

Lsid

;~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 t nl 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 CKLCCC shal IX Ilollo~tncoLs and free

lron porosity.

voids and inclusions.

9._3 Al l ) 01 the I~llown

I lll~hocs shal hc LISaI l.or

liquid steel sampling:

Ioul-ins into i.a\ . \ ul~tl~aCllll~ lllli I~;I~I\?Il-oIIIliI

i ~exl i np lron the x. l t i ; i l intensity oupLl. 111~ ~i.lcct~on

llllllt I\ ;11

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IS XXII : 1998

~~)nccnlralion Icvcls. This may Icad LOsuppression

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 ill

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~i.

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

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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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Bureau of Indian Standards

BIS

is a statutory institution established under the

Bureau of

lr7dir7r7 Stundurd

Act

1986 to promote

harmonious development of the activities of standardization, marking and quality certification of goods and

attending to connected matters in the country.

Copyright

BIS has the copyright of all its publications. No part of these publications may he reproducctl in any form

without the prior permission in writin g of BIS. This does not preclude the lrce USC. in the course 01

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

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