Bsi bs en 10136 1991 (1999)

BRITISH STANDARD BS EN 10136 1991 Chemical analysis of ferrous materials — Determination of nickel in steels and irons — Flame atomic absorption spectrometric method This European Standard EN 10136 19[.]

This European Stand rd EN1013 :19 9 has the status of a

BritishStand rd

This Bri shStan ard was

published u der the authoriy

ofthe Bo rd of BSI an comes

into fect on

3 J n ary1 9

© BSI1 -1 9

The folowing BSI references

relate to the work on this

stan ard:

Commi e reference ISM/ 18

Draft an ou ced B SI News

Ju e 9 9

ISBN 0 5 0 1 3 0 4

The European Commit e for Stand ardization, u der whose superv ision this

European Stand ard was prep red, comprises the national stand rds

org anizations of the folowing W estern European cou tries

Austria Oester eichis hes Normu g sinstitut

Belg ium Institut belg e de normalsation

Finland S omen Stand ard isoimisl to, r.y

France Association f ançaise d e normalsation

Germany Deuts hes Institut für Normu g e.V

Gre ce Helenic Org anization for Stand ardization

I eland Tech olog ical Institute of I eland

I eland National Stand ard s Authority of I eland

Italy Ente Nazionale Ital ano d i Unificazione

Luxemburg Inspection d u Trav ai et des Mines

Netherlands Nederland s Normalsatie-nstitu t

Portug al Instituto Portug uès d a Qual d ade

Sp in Asociación Esp ñola de Normalzación y Certificación

Sweden Stand rdisering skommis ionen i Sv erig e

Switz rland Association suis e d e normal sation

United King d om BritishStand rds Institution

Am endm ents is ued sinc publ cation

Amd No Date of is ue Comments

Pag e

National foreword

This BritishStand ard has be n prep red u der the d irection of the I on and Ste l

Stand rd s Pol cy Commit e It is the Eng lish lang uag e v er ion of

EN1013 :19 9 “Chemica l a na lysis o fer r ous ma ter ia ls Deter mina tion o nickel

in ste ls a nd ir ons Fla me a tomic a bsor pton spe tr ometr ic method ”,publ shed b

the European Commit e for Stand rdization ( CEN) It super ed es

BS620 -3.20.4:19 6, which is withd rawn

Other method s for the d etermination of nickel in fer ous materials hav e be n

publshed as BS620 -3.20.1 andBS620 -3.20.3

N T The te t of the EN contains the folowing minor ty og ra hical er or These ha e b en drawn

to the atenton of the a pro riate Sec etariat an wil b cor ected in the ne t edi on of the EN

In5.1.1, lines2 an 7, “a sorb ncy” should re d “a sorb nce”

In7.3.3, “Lamp cur ent — Sli width” should b directly o p sie “Folow man facturer’s

recommen atons”

In7.3.5, lines6 an 9, “a sorb ncy” should re d “a sorb nce”

In7.4,line , “v lues” should re d “v lues”

A British Stand ard d oes not purport to includ e al the neces ary prov isions of a

contract User of British Stand rd s are responsible for their cor ect a plcation

Com pl anc with a British Standard does not ofitself confer im m unity

f om leg al o l g ations

Sum mary of pag es

This document comprises a f ont cov er, an insid e font cov er, p g esi andi ,

theEN title p g e, p g es 2 to8, an insid e b ck cov er and a b ck cov er

This stand rd has be n up ated ( se copy rig ht d ate) an ma hav e ha

amendments incorporated This wi l be indicated in the amendment ta le on the

inside f ont cov er

NORME EUROPÉENNE

J nuary1 89

U C 6 9.1 :5 3.4 2:5 6.7

Ke words: Iron- an ste l prod cts, ste ls, cast iron, chemical analysis,determinaton of content, nickel, atomic a sorpton

sp ctro hotometry,flame photometry

Eng lish v er ion

Analyse chimique des matériaux

sidérurg iq ues — Dosag e du nickel d ns les

acier et les fontes Méthode par spectrométrie

d’absorption atomiq ue d ns la flamme

Chemis he Analyse v on Eisenwerkstofen—

Bestimmung von Nickel in Stahl

Flammenatomabsorptions pektrometris hes

Ver ahren

This European Stand rd was ac epted b CEN on15 J n ar y19 9 CEN

member are bou d to comply with the req uirements of the CEN/CENELEC

Rules which stipulate the conditions for g iv ing this European Stand ard the

status of a national stand rd without any alteration

Up-to-d te lsts and biblog ra hical references concerning such national

stand ard s ma be obtained on a plcation to the CEN Central Sec etariat or to

any CEN member

This European Stand ard exists in thre oficial v er ions ( Eng lish, French,

German) A v er ion in any other lang uag e ma e b translation u d er the

responsibi ty of a CEN member into its own lang uag e an notified to the CEN

Central Sec etariat has the same status as the oficial v er ions

CEN member are the national stand rd s org anizations of Austria, Belg ium,

Denmark, Finland , France, Germany , Gre ce, I eland, I eland, Italy ,

Luxemburg , Netherlands, Norway , Portug al, Sp in, Sweden, Switz rland and

UnitedKing dom

European Commit e for Stand rd ization

Comité Europé n de Normal sation

Europ is hes Komite für Normu g

Central Se retariat: rue de Stas art 3 , B- 10 0 Brus els

© CEN 19 9Copy rig ht reserv ed to al CEN member

Ref No EN 1013 :19 9E

This European Stand rd takes ov er the content of

EURONORM13 -8 “Chemical analy sis of fer ous

materials — Determination of nickel in ste ls and

irons — Flame atomic a sorption spectrometric

method ”, prep red b ECISS/TC 20 “Methods of

chemical analy sis”; the Sec etariat of which is

alocated to the Dansk Stand rdisering sra ( DS)

It has be n submit ed to the CEN Formal V ote

folowing the d ecision of the Co rd inating

Commis ion ( COCOR) of the European

Commit e for I on an Ste l Stand ard ization

on19 7-1 -24/ 25

It has be n a opted and ratified b CEN BT

on19 8-1 -0

According to the Common CEN/CENELEC Rules,

folowing cou tries are bound to implement this

European Stand rd:

Austria, Belg ium, Denmark, Finland, France,

Germany , Gre ce, I eland, I eland, Italy ,

Luxemburg , Netherlands, Norway , Portug al, Sp in,

Sweden, Switz rland an UnitedKing dom

Note in clauses1 and9 EURONORM shal rea

Contents

Pag e

7.4 Esta l shment of the calbration g ra h 5

1 Scope and field ofappl cation

This EURONORM specifies a method for the

d etermination of nickel in ste ls an irons b means

of flame atomic a sorption spectrometry

The method is a pl ca le to ste ls an irons with

nickel contents of0.0 3 to2.0% ( m/m)

2 Ref r nce

EURONORM18 — Selection and prep ration of

samples and test pieces for ste l and iron and ste l

prod ucts

General g uidelnes for the a pl cation of flame

atomic a sorption spectrometric methods are in

cour e of prep ration

3 Principle

Dis olution of a test portion in a mixture of

a propriate acids and fuming with per hloric acid

Spray ing of the solution into an air-acety lene flame

Determination of the nickel b means of the

spectrometric measurement of the atomic

a sorption of the232.0nm or3 2.5nm lne emit ed

b a nickel hol ow cathode lamp

The instrument is calbrated b a d ition of a nickel

stand rd solution to a simi ar matrix to that of the

test solution

NOT At the wa eleng th of3 2.5nm the sig nalto-noise rato

is hig her than at a wa eleng th of2 2.0nm Generaly,use of

the 5 5nm line wil le d to a b t er re rod cibiliy

Howev er, as the sensitiv ity at3 2.5nm is les than

the sensitiv ity at232.0nm,with some instruments

the use of the long er wav eleng th wi l be impos ible

when analy sing low nickel contents

4 Reag ents

During the analy sis use only reag ents of recog niz d

analy tical reag ent qual ty and hav ing a v ery low

nickel content, and only disti ed water or water of

eq uiv alent purity

Careful y check the nickel content of al reag ents

I pos ible, use only f eshly prep red disti ed or

deioniz d water

4.1 Ir on o high pur ity, with a nickel

content<0.0 0 % ( m/ m)

4.2 Hyd r ochlor ic a cid –nir ic a cid mixtur e

Mix thre v olumes of hy drochloric acid, Ô1.19g /ml

a proximately , one v olume of nitric acid , Ô1.4 g / ml

a proximately an two v olumes of water This

mixture is to be prep red immed iately before use

4.3 Nir ic a cid –per chlor ic a cid mixtur e

Mix10 ml of nitric acid, Ô1.4 g /ml a proximately

with8 0ml of per hloric acid, Ô1.5 g /ml

a proximately Di ute to1l with water and mix

NOT Perhloric acid (Ô1.6 g / ml a pro imately) ma also b

used.1 0ml of p r hloric acid (Ô1.5 g / ml a pro imately) is

e uiv lent to 9ml of p rhloric acid (Ô1.6 g / ml

a pro imately)

4.4 Nickel stock soluton, cor esponding to1 mg of

nickel per ml a proximately

W eig h, to the nearest0.0 1 g , a out0.5g of hig h

purity nickel ( W 9 9% pure) Trans er the

weig hedmas to a4 0ml beaker and dis olv e

in25ml of nitric acid [ Ô 1.4 g /ml a proximately

d iluted1 +1 ( v / v )] Boi to remov e oxides of

nitrog en Co l and trans er the solution to a5 0ml

v olumetric flask, diute to the mark with water and

mix Calculate the concentration of nickel in this

stock solution, in mg / ml

4.5 Nickel r efer enc soluton, cor esponding to4 È

of nickel per ml a proximately

Trans er10.0ml of nickel stock solution( 4.4) to

a25 ml v olumetric flask, di ute to the mark with

water and mix Calculate the concentration of nickel

in the reference solution, in Èg / ml

5 Apparatus

Ord inary la oratory eq uipment and

5.1 A tomic a bsor pt on spe tr ometer ; a nickel holow

ca thod e la mp; sup l es of air and acety lene

suficiently pure to g iv e a stea y clear fuel lean

flame, f e f om water and oi, an fe fom nickel

The atomic a sorption spectrometer used wi be

satis actory if after optimization ac ording to7.3.4

the lmit of d etection and characteristic

concentration are in reasona le ag re ment with the

v alues g iv en b the man facturer an it me ts the

folowing per ormance req uirements

5.1.1 Minimum pr ecision

The stand rd dev iation of10 measurements of the

a sorbency of the most concentrated solution shal

not exce d1.0% of the mean a sorb nce

The stand rd dev iation of10 measurements of the

a sorb nce of the least concentrated cal bration

solution ( exclud ing the z ro cal bration solution)

shal not exce d0.5% of the mean a sorbency of the

most concentrated cal bration solution

For ex mple, if the top and bot om cal bration

solutions represent0.1% and0.01 % nickel in the

sample, the precision cal ed for ( as two stand rd

dev iations) would be0.0 2% and0.0 1 % nickel

respectively , as uming curv e l nearity

5.1.2 A d d itona l per for ma nc r equir ements

It is also desira le that the instrument should

conform to the fol owing ad ditional perormance

requirements

a) Characteristic concentration — The

characteristic concentration for nickel in a matrix

simi ar to the final test solution shal be bet er

than0.10Èg /ml

b) Limit of d etection — The lmit of detection of

nickel in a matrix simiar to the final test solution

shal be bet er than0.15Èg /ml

5.2 A ncila r y equipment

A strip chart recorder and/or d ig ital read out dev ice

is recommended to ev aluate the c iteria in5.1 and

for al subsequent measurements

6 Sa mpl ng

Sampl ng shal be car ied out in ac ord nce with

W ARNING — Per hloric acid v apour ma cause

ex losions in the presence of ammonia, nitrous

fumes or org anic mat er in g eneral Alway s use a

special y desig ned fume-ho d

7.1 Test portion

W eig h the mas ( m) indicated below to the

nearest 0.0 1g: m =1 g±5%

7.2 Blank test

W ith each analy tical run, car y out an analy sis on a

reag ent blan in p ral el with the test portion

analy sis, using identical reag ents, cond itions,

analy tical procedures and d ilutions throug hout

7.3 Determ ination

7.3.1 Preparation o the te t solution

Place the test portion(7.1) in a25 ml beaker

Add10ml of hy drochloric acid nitric acid

mixture( 4.2) Heat g ently u ti the reaction ceases

Add15ml of nitric acid –per hloric acid

mixture( 4.3) and heat u ti dense white fumes of

per hloric acid a pear Contin e heating for one

minute and alow to co l

NOT If the test p rton is re dily soluble in the niric

acid–perhloric acid mixture( 4.3), the ad i on of hydrochloric

acid–niric acid mixture( 4.2) can b omi ed In that case the test

p rton is dis olv ed in the niric acid– per hloric acid

mixture( 4.3) an the soluton th s o tained is he ted as

des rib d a o e

Dis olv e in25ml of water b heating g ently Co l

ag ain and trans er the solution to a10 ml

v olumetric flask,diute to the mark with water and

mix This is the test solution I some residue has

be n left in the solution due to si con, tung sten,

niobium or tantalum, fi ter the solution throug h a

d ry , medium textured fi ter p per, dis arding the

fir t ru ning s

I the ex ected nickel content of the test sample

ex ce d s0.1 % ( m/m), diute the solution as fol ows:

Trans er25.0ml of the solution to a5 0ml

v olumetric flask,diute to the mark with water and

mix

N T If the soluton has to b diluted to g iv the test soluton,

the blan test soluton(7.2) must b diluted in the same wa

7.3.2 Prep ration o the cal b at ion solutions

Place10g of iron(4.1) in a8 0ml beaker

Add10 ml of hy drochloric acid–nitric acid

mix ture(4.2) an heat g ently to dis olv e the iron

Add15 ml of nitric acid –per hloric acid

mix ture(4.3) and heat u ti d ense white fumes of

per hloric acid a pear Contin e heating for one

min te and alow to co l Dis olv e in10 ml of

water b heating g ently Co l ag ain and trans er the

solution to a25 ml v olumetric flask, d ilute to the

mark with water and mix

7.3.2.1 Nickel content <0.1 % (m/m)

Trans er a series of25.0ml alq uots of the iron

solution to10 ml v olumetric flasks, ad d to each

flask b means of a buret e or pipet e

respectiv ely0,2.5,5.0,10.0,15.0, 20.0 and25.0ml

of nickel reference solution( 4.5), diute to the mark

with water and mix

7.3.2.2 Nickel content0.1 to2.0% (m/ m)

Trans er25.0ml of the iron solution to a5 0ml

v olumetric flask,d ilute to the mark with water and

mix From this solution trans er25.0ml al q uots

to10 ml v olumetric flasks

Ad d to each flask b means of a buret e or pipet e

respectiv ely0,2.5,5.0,10.0,15.0, 20.0 and25.0ml

of nickel reference solution( 4.5), diute to the mark

with water and mix

N T 1ml of nickel reference soluton( 4.5) is a pro imately

e uiv lent to0.0 4% ( m/ m) in the sample in the case of7.3.2.1

an 0.0 % ( m/m) in the sample in the case of7.3.2.2

7.3.3 Adjust ment o at omic abso ption

spe t rometer(5.1)

NOT The man facturer’s recommen atons should b closely

folowed an p rtcular atenton is drawn to the folowing safety

p ints:

a) the e plosiv e nature of acetylene an reg ulatons

concerning is use;

b) the ne d to shield the e es of the o erator fom UV

radiaton b me ns of tnted g las ;

c) the ne d to ke p burner he d cle r of de osis.A b dly

clog g ed burner ma cause a flash b ck;

d) make sure that the liquid tra is filed wih water

7.3.4 O ptimizat ion o the atomic abso ption

spe t romet er s tt ings

Fol ow the man facturer instructions for

prep ring the instrument for use

W hen the cur ent to the lamp, the wav eleng th an

flow of g as hav e be n a justed and the burner l t,

spra water u ti the indication has sta i z d Set

the a sorb nce v alue to z ro Cho se a d mping

set ing or integ ration time to g iv e a sig nal stea y

enoug h to fulfi the precision req uirements( 5.1)

Adjust the flame to be clear fuel lean and the

burnerheig ht to a out1cm below the l g ht p th

Spray ing , alternately , the hig h and z ro

calbrationsolutions, a just the g as flow and

burnerposition ( horiz ntaly , v ertical y and

rotationaly ) u ti the diference in a sorb nce

betwe n the cal bration solutions is at a ma imum

Ev aluate the c iteria of5.1.1 to ensure that the

instrument is suita le for the determination

7.3.5 At omic abso ption measurement s

Set the s ale ex ansion so that the top calbration

solution g iv es nearly ful s ale deflection Aspirate

the calbration solutions in as end ing order

repetitiv ely unti each g iv es the ac epta le precision

( se 5.1.1), thus showing that the instrument has

achiev ed sta i ity Select two cal bration solutions,

one hav ing an a sorbency just lower than the test

solution an one just hig her Aspirate these fir t in

as end ing ord er, then in des end ing ord er, with the

test solution as the mid le solution in each case,

measuring the a sorbency in relation to water

Aspirate the complete rang e of calbration solutions

ag ain

It is recog niz d that these procedures can ot be

folowed with automatic instruments which ac ept

two cal bration solutions only In this case, it is

sug g ested that the two “ sandwiching ” solutions

should not be used for the primary calbration but

should be analy sed alternately with the test

solution

Obtain the net mean a sorb nce of each calbration

solution b subtracting the mean a sorb nce of the

z ro cal bration solution

Obtain the mean a sorb nce of the test solution and

the mean a sorb nce of the reag ent blan solution

Conv ert the mean a sorb nces of the test solution

and of the reag ent blan solution to mic og rams of

nickel per mi l itre b means of the calbration

g ra h(7.4)

7.4 Esta l shm ent of the cal bration g ra h

It is neces ary to draw up a new calbration g ra h

for each series of determinations, and for the rang e

of nickel contents ex ected

Prep re a cal bration g ra h b plot ing the net

mean a sorb nce v elues of the calbration solutions

ag ainst mic og rams ofnickel per mi i tre,

calculated ac ording to4.5 Refer the net

a sorb nces of the two a jacent cal bration

solutions to the g ra h I these two calbration

rea ing s do not d ev iate fom the g ra h b more than

the permit ed precision c iteria then the test

solution rea ing s are ac epta le

8 Expres ion ofresults

The per entag e b mas of nickel ( Ni is g iv en b the

ex res ion

Ty pe of lamp: Nickel hol ow cathod e

W aveleng th: 232.0nm or3 2.5nm

Flame: Air-acety lene clear fuel ean

flame ad justed for ma imum

Lamp cur ent —

Slt width

nickel response

Folowmanufacturer’s

recommend tions

where:

b is the concentration of nickel in the test

solution inÈg /ml;

c is the concentration of nickel in the reag ent

blan solution inÈg /ml;

D is the di ution factor in7.3.1;

( D =1 for samples with an ex ected nickel

content of0.1 % or les ,

D =20 for samples with an ex ected nickel

content of more than0.1%);

m is the mas of the test portion, in g

Ni % ( m/m)

b–c ( )⋅D⋅10

10 6

10

m

b–c ( )⋅D

=

⋅

=

9 Test r port

The test report shal contain the fol owing

p rticular :

a) The method of analy sis used b reference to

this EURONORM;

b) the results obtained, as wel as the form in

which they are ex res ed ;

c) any p rticular detai s which ma hav e be n

noted during the d etermination;

d ) any operations not specified in this

EURONORM or any optional operations which

could hav e ha an influence on the result;

e) al indications neces ary for the id entification

of the sample;

f) the la oratory and the d ate of analy sis