Bsi bs en 10276 2 2003

BRITISH STANDARD BS EN 10276 2 2003 Chemical analysis of ferrous materials — Determination of oxygen content in steel and iron — Part 2 Infrared method after fusion under inert gas The European Standa[.]

Chemical analysis of

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ICS 7 0 0.3

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EN1027 -2:20 3

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ISE/18, Samplng and analysis or iron and ste l, which has th e responsibi ity

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N ORM E EU ROPÉEN N E

July 2 0

ICS 7 0 0.3

En ls ver sion

Chemical analysis of fer rous mater ials - Deter mination of oxygen

content in steel and iron - Part 2: Infr ared method af er fusion

under iner t gas

A naly e c imiq e d s maté a x fer re x - Déter min tio d

la te e r e o y è e d la ier et d la fo te - Partie 2:

Méth d p r a s r ptio d n lnfr ar ou e a r ès fu io s u

g z in r te

Ch mis h An ly e v n Eis nwer k stofe - Be timmu g

d s Sa er stofg h lts v n Sta l u d Eis n - Tei 2:

Me s n d r Infrar ota s rptio n c Aufs hmelz n u ter

In r tg s

This Eur op a Sta d r d w as a pr ov d b CEN o 7 Ma 2 0

CEN memb rs ar e b u d to c mply w ith th CEN/CENELEC Inter nal Re ulatio s w hic stip late th c n itio s for givin this Eur op a

Sta d rd th statu of a n tio al sta d r d w ith ut a y alteratio Up-o-d te lsts a d biblo ra hic l r efer en e c n ernin s c n tio al

sta d r ds ma b o tain d o a plc tio to th Ma a eme t Ce tre or to a y CEN memb r

This Eur op a Sta d rd e ists in thr ee oficial v r sio s (En ls , Fre c , Ger ma ).A v r sio in a y oth r la g a e ma e b tr an latio

u d r th r es o sibi ty of a CEN memb r into its own la g a e a d n tifie to th Ma a eme t Ce tr e h s th s me statu a th oficial

v ersio s

CEN memb r s are th n tio al sta d rd b die of Au tr i ,Belgium, Cz c Re u lc, De mar k,Finla d, Fr an e,Germa y,Gre c ,

Hu g r y,Ic la d, Ir ela d,Italy, L x mb ur g, Malta, Neth r l n s,Nor wa , Portu al Slo akia,Sp in, Sw ed n,Sw itz rla d a d Unite

K in d m

E U R OPE A N COMMITT E E FO STA N DA R DI Z A TION

COMIT EUROPÉ N DE NORMALISATION

EUROPÄISCHES K MIT E FÜR N RMUNG

Management Cente:rue de Sta s r, 3 B-10 0 Brus els

Foreword .3

1 Sc pe 4

2 Normativ refere c s 4

3 Prin iple .4

4 Re g nts a d materials 4

5 Apparatu 6

6 Sampln 6

7 Pro e ure .7

7.1 Ge eral 7

7.2 Ge eral instru tio s 7

7.3 Te t portio 7

7.4 Bla k te t 7

7.5 Cal bratio 8

7.6 Preparatio te t .8

7.7 Determin tio 8

7.7.1 Meth d 1 8

7.7.2 Meth d 2 8

8 Expre sio of re ults 9

8.1 Meth d of c lc latio 9

8.2 Pre isio 10

9 Te t report .12

Bibl o raph 13

This doc ment EN 10 7 -2:2 0 has b en pr ep red by Tec nical Commite ECISS/TC 2 “Method of

c emical analy sis of ferou prod cts”, the secretariat of whic is held by SIS

This Eur op an Stan ard s al b given the statu of a national stan ard, either by publcation of an identical

text or by en orsement, at the latest by Jan ary 2 0 , an conflctin national stan ard s al b with r awn at

the latest by Jan ary 2 0

This doc ment in lu es a Biblogr aphy

Ac or din to the CEN/CENELEC Internal Reg lation , the national stan ard organization of the folow in

cou tries are b u d to implement this Euro e n Stan ard: Au tr ia, Belgium, Czec Re ublc, Denmark,

Finlan , Fran e, Germany, Gre ce, Hu gary, Icelan , Irelan , Italy , Lu emb ur g, Malta, Netherlan s,

Norway , Portu al, Slov akia, Sp in, Sweden, Switzerlan an the United K in dom

1 Scope

This Euro e n Stan ard sp cifies an infrar ed method afer fu ion u der iner t gas for the determination of

oxygen in ste l an iron

The method is a plca le to oxy gen contents b twe n 0,0 0 % (m/m) an 0,01 % (m/m)

This Euro e n Stan ard in orp rates by dated or u dated refer en e, provision fr om other publcation

These normative r efer en es ar e cited at the a pro r iate places in the text, an the publcation ar e lsted

here fer For dated referen es, s bseq ent amen ments to or rev ision of an of these publcation a ply to

this Euro e n Stan ar d only when in or porated in it by amen ment or revision For u dated referen es the

latest edition of the publcation r eferr ed to a ples (in lu in amen ments)

in ste l an iron – Part 1: Sampln an pre aration of ste l

samples for ox gen determination

determination of c emical comp sition (ISO 14 8 :19 6)

3 Principle

Fu ion of a test p rtion in a sin le-u e gra hite cr ucible u der helum gas at a minimum temp r ature of

2 0 ° C Combination of the oxygen from the sa mple w ith car bon from the cr ucible to for m carb n monoxide

Eventualy tran formation of carb n monoxide into carb n dioxide

Me s r ement of infr ared a sor ption of the car bon monoxide or dioxide an u e of a calbration c rve ploted

u in the me s rements o tained w ith p tas ium nitr ate

Durin the analy sis, u les otherw ise stated, only re gents of recog ised analy tical grade s al b u ed The

folow in re gents an materials s al b u ed:

4.1 Hel um, hig purity , total impurity content 0,0 0 % (m/m)

An oxidation catalyst [co p r (I) oxide or platin m] tub he ted to a temp rature a ove 4 0 °C s al b u ed

pr ior to a purify in u it, w hen the presen e of organic contaminants is s sp cted in the helum

4.2 Ma ne ium perchlor ate, Mg (ClO

4 )

2 , (commer cial desig ation: an y dr one), p rticle size from 1,2

mm to 2,0 mm, or Anhy drous Calcium sulphate, (CaSO

4 ), (commercial desig ation: drierite), p rticle

size from 0,6 mm to 0,8 mm

4.3 Sodium hydroxide on gra ulate s pport, (NaOH), (commercial desig ation: as arite), p rticle

size from 0,7 mm to 1,2 mm

4.4 Copper oxide, CuO

4.5 Platinum, Pt

4.6 Tin or nick el ca s le , For exa mple ∅ 5 mm, len th 13 mm, weig t 16 mg, w ith low oxy gen content,

les than 0,1 µg/mg of oxygen

Cut of the up er p rt of the tin ca s le to red ce the w eig t to 5 mg or the len th to 8 mm

4.7 W ater , high purity, deionized, pre ared ju t b fore u e

4.8 Pota sium nitrate, KNO3, hig purity , maximum total impurity content 0,0 0 % (m/m)

Dry b fore u e at 10 °C to 10 °C for 2 h an alow to co l in a des icato

4.9 Pota sium nitrate stoc s lution, cor resp n in to 4 mg/ml of oxy gen

Weig , to the ne rest 0,1 mg, 8,416 g of p tas ium nitrate (4.8)

Place in a 10 ml b aker an dis olve in a out 5 ml of w ater (4.7)

Tr an fer q antitatively to a 10 0 ml volumetr i flas , diute to the mar k w ith w ater (4.7), an mix

1 ml of the p tas ium nitr ate stoc solution contain 4 mg of oxy gen as p tas ium nitrate

4.10 Pota sium nitrate di ute stoc solution, cor resp n in to 0,4 mg/ml of oxygen

This solution s al b pr ep red fres ly b fore u e

Tran fer 10 ml of the p tas ium nitrate stoc solution in a 10 ml volumetric flas , diute to the mark w ith

water (4.7), an mix

1 ml of the p tas ium nitr ate stoc solution contain 0,4 mg of oxygen as p tas ium nitrate

4.1 Pota sium nitrate sta dard solutions

These solution s al b pre ared fres ly b for e u e

Tran fer the volume lsted in Ta le 1 of the p tas ium nitrate stoc solution (4.9) an of the p tas ium nitrate

diuted stoc solution (4.10) in a series of nine 10 ml v olumetr i flask s, diute to the mar k w ith water (4.7),

an mix

10 µl of e c of the p tas ium nitrate stan ar d solution contain the mas of oxygen (as p tas ium nitrate)

lsted in the last column of Ta le 1

Table 1 — Pota sium nitrate sta d rd s lutio s

Pota sium nitrate

sta dard s lutio

Volume of pota sium

nitrate sto k s lutio

(4.9) a d d

(e c pt for solution 4.1 2)

Ma s of o y ge in

1 ml of th

pota sium nitrate

sta d rd s lution

Ma s of o y ge in

10 µl of th

pota sium nitrate

sta d rd s lutio

a

0 mg

0 µg

4.1 2 3 ml of p tas ium nitrate

diuted stoc solution

(4.10)

0,012 mg

1,2 µg

4 µg

8 µg

12 µg

12 µg

a

zero memb r: The stan ar d solution (4.1 1) is in fact the w ater (4.7) u ed for pre arin the

solution

4.12 Graphite powder, hig purity, w ith low oxy gen content

The a p ratu req ir ed for fu ion of the test p r tion an me s r ement of the carb n monoxide or dioxide

extracted may b o tained commercialy from a n mb r of man facturer s The man facturer's in tru tion for

the o eration of the in trument s al b folow ed

5.1 Gra hite crucible, sin le-u e

Hig purity cru ibles s ited to the a p r atu s al b u ed

5.2 Crucible tongs s al b u ed for han ln the cr ucibles

5.3 Gla s wool fi ters

5.4 Micropipet e, 10 µl, s al b u ed, lmit of er ror s al b les than 1 µl

Sampln s al b caried out in ac ordan e with EN ISO 14 8 an EN 10 7 -1

7 Procedure

The ris inv olv ed when u in an a p ratu for fu in the test p r tion ar e mainly r i k of burn Cr ucible ton s

(5.2) an a pro r iate container s for the u ed cru ibles s al b u ed

7.2 Ge eral instructions

It s al b c ec ed that glas wo l fiters (5.3) are cle n an they s al b c an ed as ofen as neces ary

If the electricity s p ly has b en sw itc ed of for a lon time, the in tr ument s al b alow ed to sta i se for

the time recommen ed by the man facturer

Afer c an in the fiters (5.3) an /or r eagents (4.2, 4.3 an 4.4), or when the a p ratu has b en ino erative

for a p riod, the in trument s al b alowed to sta i se by car y in out trial analyses, the res lt of w hic are to

b disr egarded, then pr oce d w ith blan calbration an pre aration tests as in icated in 7.4, 7.5 an 7.6

b fore analysin the sample

If the in trument u ed prov ides a dir ect re din in p rcentage of oxy gen, the in trument re din s al b

adju ted for e c calbration r an e as folow s:

Usin a CRM w ith a hig oxy gen content, r ecord the contents me s red at diferent levels of furnace he tin

p w er The req ired he tin p w er for the deter mination of test samples is that at whic the re din levels of

In order to determine a hig aloy test sample, a hig aloy CRM s al b u ed to k ow the req ir ed he tin

p w er

7.3 T est portion

Pr ep r e the test p rtion of a pr oximately 1 g in ac or dan e w ith EN 10 7 -1

Weig the test p rtion to the ne rest 1 mg

7.4 Blank te t

Pr ior to the determination, the folowin blan test s al b car ried out in d plcate

Pr oce d as in 7.7 w ithout test p rtion, enterin a weig t of 1 g, an setin the blan s btr action of the

in tr ument to zero

Obtain the re din of the blan test

The me n value of the blan test s al b s ficiently low when comp r ed to the ox gen content to b

determined in the test p rtion

For me n values b low 8 µg/ g of oxy gen, neither the me n blan v alue nor the difer en e b twe n the tw o

blan v alues s ould ex e d 0,5 µg/ g of oxy gen For me n values a ove 8 µg/ g of oxygen, neither the me n

blan value nor the difer en e b tw een the tw o blan values s ould ex e d 2 µg/ g of oxy gen

If the blan v alues are a normaly hig , the sour ce of contamination s al b inv estigated an elminated

If the me n value of the blan is satisfactory, it may then b introd ced in the blan s btr action device of the

in trument

7.5 Cal bration

Pr ior to the deter mination, the folowin calbration s al b caried out

Pr ep r e ac or din to 4.1 at le st five solution c osen from solution 4.1 1 to 4.1 9 in icated in Ta le 1,

ac ordin to the level of oxy gen content to b deter mined

Usin the micro ip te (5.4), tr an fer 10 µl of e c of the fres ly pr ep red p tas ium nitr ate stan ar d

solution (4.1 1 to 4.1 9) to e c tin or nic el ca s le (4.6) resp ctiv ely an dry at 9 °C to 9 °C for 2 h

NOT E T he dr yin of th calbrat io solutio s in th t in or nick el ca sules sh uld b d n ste wise, in ord r to av oid

spla shin a d los of ca libratio material d e to ov er -ra pid h at in b f ore complet e v ap ri at io of t he water

Carefuly pr es the tin or nic el ca s le an pr oce d as in 7.7, u in the tin or nic el ca s le as a test p rtion,

enterin a sample weig t of one gr am, an setin the sample fu ion temp rature to 2 0 °C to lmit tin

v ap r i ation

Pr ep re a calbration gra h by plotin the re din o tained fr om the in trument again t oxy gen content

expres ed in microgra ms fr om the last column of Ta le 1

Pr ior to the determination, the folowin pre aration test in d plcate s al b carr ied out

Cho se a CRM or routine sample ( o b pre ared ju t b fore deter mination) with an oxy gen content close to

that exp cted in the samples to b analysed

Pr oce d as in 7.3 for the pre ar ation of this prelminary sample

Pr oce d as in 7.7 for the determination on the prelminary sample

The r es lts s al b w ithin the lmits of a contr ol c art for the prelminary sample

If not, c ec the pre aration con ition an re e t the sample pre aration test

7.7.1 Meth d 1

The electr ode s al b cle ned w ith a bru h an vac um cle ner b fore e c deter mination

Place a gra hite cr ucible (5.1) in the furnace an then degas by he tin a ov e 210 °C to 2 0 °C

Afer a co ln p riod of five to ten secon s, put the test p r tion with an empty tin or nic el ca s le (4.6) into

the degas ed cru ible, enterin a sample w eig t of one gram

Analy se in ac or dan e w ith the a p ratu man facturer ' in tru tion

At the en of the fu ion an me s rin cy cle, r emove an dis ard the cr ucible an r ecord the value display ed

by the analyser

7.7.2 Meth d 2

The electr ode s al b cle ned w ith a bru h an vac um cle ner b fore e c deter mination

Place a gra hite cru ible (5.1) in the furnace an then degas by he tin a ov e 210 °C to 2 0 °C Re e t

degas in on e if p s ible with the a p ratu u ed