Tiêu chuẩn iso 11114 4 2017

The work of pr p ring Int ernational Stan ards is normaly car ied out through ISO t ech ical committ ees.. The proc d r s used t o develo this document an those int en ed for it furthe m

Transportable gas cylinders —

Part 4:

B outeille s à g z tra sporta le s — Comp tibilité de s matériau et des

ro inet a e le s co ten s g zeu —

Partie 4 : Méth de s d’e ssai p ur le ch ix des aciers résista t à la

fra ilisation p r l’h dro ène

COPYRIGHT PROTECTED DOCUMENT

© ISO 2017, P blshed in Sw itz rlan

A ll rig hts r eserved Unles otherw ise spe ified, nopar of this p blc tion ma y be r epr od c d or utilz d otherw ise in an form

or b an me ns, ele tr onic or me hanic l, inclu in p oto opying , or postin on the internet or an intranet , w ithout prior

written permis ion Permis ion c n be req esed from either ISO at the ad r es below or ISO’s member bod y in the c u try of

F reword i v

Introduction v

1 Sc ope 1

2 Nor mati ve r eferenc es 1

3 Terms, definitio s, symbols and abbr eviated ter ms 2

3.1 Te msan definitions 2

3.2 Symb ls and a br eviated te ms 3

4 General r equirements 3

5 Test metho s 4

5.1 Disc tes (method A ) 4

5.1.1 Principle of tes 4

5.1.2 Tes con itions an pr oc dur e 4

5.1.3 Tr eatment an inte pr etation of tes r esult 6

5.1.4 Faiur e in con ucting tes 7

5.1.5 Tes report 7

5.2 Fracture me hanics tes (method B) 1

5.2.1 Principle of the tes method 1

5.2.2 Tes pr oc d r e 1

5.2.3 Tes results 14

5.3 Tes method to dete mine the r esis anc to hydr og en as is ed cracking of s e l cyln e s (method C) 14

5.3.1 General 14

5.3.2 Spe imen config urations and numbe s of tes s 1

5.3.3 Fatig ue pr ecracking 1

5.3.4 Spe imen testing pr oc dur e 1

5.3.5 Tes pr oc d r e

1 5.3.6 Crack g r owth examination 1

5.3.7 C ln e mate ial q alfication 1

5.3.8 Faiur e in con ucting tes 1

5.3.9 Tes report 1

5.4 Tensie tes s 1

Biblog raphy 18

ISO (he Int ernational Org nization for Stan ardization) is a worldwidefede ation of national s an ards

b dies (ISO membe b dies) The work of pr p ring Int ernational Stan ards is normaly car ied out

through ISO t ech ical committ ees Each membe b dy int er st ed in a subje t for w hich a t ech ical

committ ee has be n es a lshed has the right t o be r pr sent ed on that committ ee Int ernational

org nizations, g overnmental an non-g ove nmental, in laison with ISO, also take part in the work

ISO cola orat es closely with the Int ernational Ele trot ech ical C mmis ion (IEC) on al matt ers of

ele trot ech ical s an ardization

The proc d r s used t o develo this document an those int en ed for it furthe maint enanc ar

desc ibed in the ISO/IEC Dir ctives, Part 1 In p rticular the dife ent a pro al c it eria ne ded for the

dife ent ty es of ISO document should be not ed This document was draft ed in ac ordanc with the

edit orial rules of the ISO/IEC Dir ctives, Part 2 ( e www iso org dir ctives)

A tt ention is drawn t o the p s ibi ity that some of the element of this document ma be the subje t of

p t ent right ISO shal not be held r sponsible for identifying any or al such p t ent right Detais of

any p t ent right identified d ring the develo ment of the document wi be in the Introd ction an / r

on the ISO ls of p t ent de larations r c ived ( e www iso org p t ent )

Any trade name used in this document is information given for the convenienc of use s an does not

cons itut e an en orsement

For an ex lanation on the meaning of ISO spe ific terms an ex r s ions r lat ed to conformity as es ment,

as wel as information a out ISO’s adhe enc to the Wor ld Trade Org nization (WTO) principles in the

Te h ical Bar ie s to Trade (TBT) se the folowing URL: www iso org iso/ for word html

The committ ee r sp nsible for thisdocument is ISO/TC5 , G as cylnde s

This se on edition canc ls an r plac s the f irs edition (ISO 1 1 4-4:2 0 ), w hich has be n

t ech icaly r vised with the folowing chang es:

— impro ement of the proc d r cor esp n ing t o Method Can adjus ment of ac eptanc c it eria;

— l ght modifications on proc d r s cor esp n ing t o Method A an Method B

A l s of p rt in the ISO 1 1 4 se ies can be fou d on the ISO websit e

It is widely r co niz d that compr s ed hydrog en an some hydrog en bearing g ses can ha e an

embrit lng efe t on st eels Thisembrit lng efe t has r sult ed in the fai ur of hydrog en g s cy lin e s

( inclu ing someburs s)that hasled g s cy lin e use s an man factur rs t o ado t pe ific measur s

The ado tion of these measur s has elminat ed al k own faiur s of hydrog en cy lin e s from this

embrit lement phenomenon as far has be n r p rt ed

The b sic r commen ation is t o lmit the t ensie s r ngth of the st eels ( e ISO 1 1 4-1) an el minat e

man facturing defe t

This t ensie s r ngth l mit of 9 0 MPa was develo ed for q enched an t empe ed g s cy lin e s of

34 Cr Mo 4 ty e st eels using st eelmaking practic s, chemis ry an man facturing t ech iq es ty ical

of those used d ring the early 1 80’s an suc es fuly used for fil ing pr s ur s up t o 3 0 b r This

practic has be n in widescale use up t o the cur ent time Othe highe pr s ur s, although at lowe

t ensie s r ngth l mit , ha e also be n used

In r c nt years, impro ement in st eelmaking, e.g b r d cing the sulph r an phosphorus cont ent ,

ha e in icat ed the p s ibi ty of inc easing the t ensie s r ngth lmit of 9 0 MPa for embrit l ng g s

se vic Ex e imental work has shown that the r lev nt p ramet ers afe ting hydrog en embrit lement

ar the folowing:

a) mic os ructur r sulting from the combination of the chemis ry an the heat tr atmen

b) me hanical pro e ties of the mat erial;

c) a pled s r s ;

d) int ernal surfac impe fe tions r sulting in local s r s conc ntrations;

e) charact eris ics of the g s contained (composition, q al ty, pr s ur , et c )

When develo ing this document, only the mat erial aspe t , a) an b) an the charact eris ics of the

g s e) a o e, we e conside ed Othe es ential featur s, c) an d), ar co e ed b the r lev nt part of

ISO 9 0

Some low alo st eels othe than 34 Cr Mo 4 ma r q ir t ensie s r ngth t o be lowe than 9 0 MPa, or

ma be pe mitt ed t o be highe than 9 0 MPa, t o be suita le for the man factur of g s cy lin e s for

embrit lng g s se vic

This document spe if ies t es methods t o identify st eels w hich, w hen combined with the cy lin e

man facturing r q ir ment spe if ied in ISO 9 0 (al part ), wi l r sult in cy lin e s suita le for use in

embrit lng g s se vic

These t es s ha e be n develo ed fol owing an ext ensive world-wide pro ramme w hich incorporat ed

la orat ory an ful scale t es s S e also AFNOR FD E2 -7 3

Transportable gas cylinders — Compatibility ofcylinder

Part 4:

This document spe if ies t es methods and the ev luation of r sult from these t es s in orde t o q al fy

st eels suita le for use in the man factur of g s cy lin e s (up t o 3 0 0 l) for hydrog en an hydrog en

bearing embrit lng g ses

This document only a ples t o seamles st eel g s cy lin e s

The r q ir ment of this document ar not a plca le if at leas one of the fol owing con itions for the

int en ed g s se vic isfulfil ed:

— the working pr s ur of the fil ed embrit lng g s is les than 2 % of the t es pr s ur of the

cy lin e ;

— the p rtial pr s ur of the f iled embrit lng g s of a g s mixtur is les than 5 MPa (5 b r) in the

case of hydrog en an othe embrit lng g ses, with the ex ception of hydrog en sulphide an methy l

me ca tan; in such cases, the p rtial pr s ur shal not ex ce d 0,2 MPa (2,5 b r)

NOTE In such cases, it is pos ible to design the cylin er as for ordinary (non-embrit ling)g ses

2 Normati ve r eferences

The folowing document ar r fe r d t o in the t ext in such a wa that some or al of their cont ent

cons itut es r q ir ment of this document F or dat ed r fe enc s, only the edition cit ed a ples F or

un at ed r fe enc s, the lat es edition of the r fe enc d document ( inclu ing any amen ment ) a ples

ISO 7 3 -1, Cor os ion o metals a d aloys — Str s s c or os io tes tin — Part 1: G ene al g ida c e o tes tin

proc edur s

ISO 7 3 -6:2 1 , Cor os io o metal s a d alo s — Str s s c orros io tes tin — Part 6 : Prep ratio a d us e

o pr c racked s pec imens fr tes ts u de c ons ta t lo d or c ons ta t di s plac ement

ISO 9 09-1, G as cylnde s — R efi a le s eamles s s te l g s cylnde s — Des ig , c ons truc tion a d tes tin —

Part 1: Quenched a d tempe ed s te l cylnde s w ith tens ile s tr n th les s th n 110 MPa

ISO 9 09- 2, G as cylnde s — R efi a le seamles s s te l g s cylnde s — Des ig , c ons truc tio a d tes tin —

Part 2 : Quenched a d tempe ed s te l cylnde s w ith tens ile s tr n th gr ate th n or eq al to 1 10 MPa

ISO 1 1 4-1:2 1 , G as cylnde s — Comp tibi t y o cylnde a d v lve mate ial s w ith g s c ontents —

Part 1: Metal c mate ial s

ISO 1 1 0, G as cylnde s — R efi a le s eamles s s te l tu es o wate c ap c it y bet we n 150 l a d 3 0 l —

Des ig , c ons truc tio a d tes tin

3 Terms, definitions, symbols and abbr eviated ter ms

3.1 Terms and definitions

F or the purp ses of this document, the folowing t erms an definitions a ply Some of the def initions

used ar b sed upon those in ISO 7 3 -1 an ISO 7 3 -6

ISO an IEC maintain t erminolo ical data ases for use in s an ardization at the folowing ad r s es:

• IECEle tro edia: a aia le at ht p:/ www ele tro edia org

• ISO Onlnebrow sing plat orm:a ai a le at ht p:/ www iso org o p

3.1.1

embrit l ng g ses

g ses w hich can cause c acking of metal d e t o the combined action of s r s and hydrog en at oms

Not e 1t o entry: Embrit ling g ses are list ed as grou s 2 an 1 in ISO 1 1 4-1:2 1 , A.4

hy rog en embrit lement index

ma imum v lue of theratio P

He/P

H2

as a fu ction of the pr s ur rise rat e

3.1.5

environmentaly-as isted c acking

syne gis ic efe t on a metal ca used b the simultaneous action of a p rticular environment an a

nominal y s atic t ensi e s r s , w hich r sult in the formation of c acking

fu ction of a pled lo d, c ack length an spe imen g eometry ha ing dimensions of s r s × leng th

w hich uniq ely def ine the elas ic -s r s f ield int ensif ication at the tip of a c ack subje t ed t o o ening

mode displac ment (mode I)

s r s int ensity fact or a o e w hich an environmentaly-as ist ed c ack wi l initiat e an grow, for

the spe if ied t es con itions un e con itions of high cons raint t o plas ic deformation, i.e un e

es entialy plane s rain con itions

3.2 Symbols and abbr eviated terms

a efe tive c ack length measur d from the c ack tip t o the lo ding plane

mean disc thick es

E mod lus of elas icity

thr shold s r s int ensity fact or

m elas ic displac ment pe unit lo d

theor tical helum ruptur pr s ur cor esp n ing t o the same pr s ur rise rat e as for the

hydrog en t es , calculat ed b r gr s ion from the cor e t ed helum ruptur pr s ur

R

m

actual v lue of t ensie s r ngth

V c ack-mouth o ening displac ment (CMOD ) defined as the mode 1 (also caled o ening -mode)

comp nent of c ack displac ment d e t o elas ic an plas ic deformation, measur d at the

location on a c ack surfac that has the gr at es elas ic displac ment pe u it lo d, m

W efe tive width of a comp ct spe imen, measur d from the b ck fac t o the lo ding plane

Y s r s int ensity fact or coeff icient de ived from the s r s analy sis for a particular spe imen

g eometry, w hich r lat es the s r s int ensity fact or for a given c ack length t o the lo d an

spe imen dimensions

HAC hydrog en as ist ed c acking

4 General r equir ements

The t es methods as desc ibed in Clause 5 ar v ld for al designed working pr s ur s The t es shal

be pe formed at ro m t empe atur at not les than the designed working pr s ur Al t es s shal be

con uct ed t o ev luat e the hydrog en embrit lement taking int o ac ount conditions that wi l be fou d in

the int en ed a plcation The comp sition of the t est ed g s shal ha e a conc ntration of embrit l ng g s

not les than the ma imum conc ntration in the int en ed a plcation The t es s shal be pe formed for

sele ting st eelsfor hydrog en/embrit lng g ses an mixtur s cy lin e s Chromium-moly bden m st eels,

q enched an t empe ed with a guarant eed ma imum actual ultimat e t ensie s r ngth of 9 0 MPa,

do not ne d t o be t est ed an can safely be used for the cons ruction of hydrog en/embrit lng g ses

cy lin e s;howeve , H

2

S mixtur s at mor than 1 0 b r working pr s ur ne d t o be t est ed F or carb

n-mang nese st eels, dife ent l mit on ultimat e t ensies r ngth a ply (as desc ibed in ISO 9 09-1)

The t es s desc ibed in Clause 5 ar “q al f ication t es s” for a given st eel composition an heat tr atment

This means that the t es s ne d not be r peat ed for each ty e, as def ined in ISO 9 0 (al p rt ), of

cy lin e onc a st eel has be n q alfied for a spe if ic design s r ngth level

The t es samples shal be taken from a r pr sentative cy linde or from a pie e of tube (for long

cy lin e s, ac ording t o ISO 1 1 0), r pr sentative of the r lev nt man facturing proc s inclu ing heat

tr atment

The t es samples shal ha e a me hanical s r ngth not lowe than the ma imum int en ed t ensie

s r ngth t o be used for the cy lin e s t o be man factur d If it isint en ed lat er t o inc ease the ma imum

s r ngth of the st eel, a new q alf ication t es shal be pe formed

W ith r spe t t o the p s ible v riation of the chemical comp sition, the chemis ry of the st eel t est ed shal

be r corded in the q al f ication t es r p rt an the dife enc in chemis ry for the st eels actualy used

for the cy lin e s shal not ex ce d the “ pe mis ible dife enc ” ac ording t o ISO 9 0 - 2 In ad ition, for

sulph r an phosphorus, these pe mis ible dife enc s ar lmit ed t o 0,00 % an 0,0 0 %, r spe tively

In no case shal the phosphorus cont ent of eithe the q alf ication or the prod ction cy lin e s ex ce d

0,0 5%

W ith r spe t t o the heat tr atment, the man factur r shal spe ify the r lev nt t empe atur s an

times, an the q enching con itions( if r lev nt) Any modification t o the heat tr atment ne ding a new

ty e a pro al ac ording t o ISO 9 0 - 2 r q ir s a new q alf ication t es

F or the q alf ication of a given st eel for the man facturing of g s cy lin e s, method A, B, or C can be

used ( e 5.1, 5.2and 5.3, r spe tively) Ad itionaly, t ensiet es s shal be car ied out se 5.4)

5.1 Dis test (method A )

5.1.1 Pr inciple of test

A mount ed t es pie e in the sha e of a disc is subje t ed t o an inc easing g s pr s ur at cons ant rat e

t o burs or t o c ack The embrit lng efe t of hydrog en (or othe embrit l ng g s) is evidenc d b

comp ring the hydrog en ruptur pr s ur s, P

H2, with the hel um ruptur pr s ur s, P

He, helum being

The lowe the ratio, the les susc ptible the st eel wi be t o embrit lement This ratio is depen ent on

the pr s ur rise rat e, w hich shal r main cons ant d ring the w hole t es

NOTE Hydro en/ mbrit ling g ses ru ture pres ures also depen on the hydrog en p rity Oxy gen or traces

of water vapour can partial y in ibit he hydro en embrit lement efect

5.1.2 Test c onditio s and pr oc edur e

5.1.2.1 S mple dis

The sample disc shal be flat an grou d (or machined t o an eq iv lent surfac f inish), an shal ha e

the folowing charact eris ics

— thick es :0,7 mm ±0,0 mm;

— flatnes : les than 1/ 10 mm defle tion

NOTE 1 T e hydro en ru ture pres ures are in the rang e of 3 0b r If it is int en ed t o evaluate the st eel for

higher working pres ure, thick es higher than 0,75 mm can b used

NOTE 2 F or g ses int en ed t o b used at ma imum working pres ure les than 1 0 b r, the test results could

b conservative In such case, the t est could b repe ted with disk at hick es such that he failure pres ure is

no more than service pres ure

Surfac con ition (b th sides):

— rough es :R a v lue ( e ISO 42 7) les than 0,0 1 mm; the rough es of the samples used for b th

H

2

an He t es sshal be eq iv len

— no visible o ides

The folowing o e ations shal be pe formed t o ve ify the sample q alty

— Immediat ely aft er the final pr p ration an prior t o the t es ing, st or the samples in a dry

atmosphe e, i.e a desic at or

— Degr ase the sample an che k thicknes at 4 p int taken 9 ° a art t o define a mean thick es

— Det ermine the disc’s hard es (e.g V ickers) o e it out er cir umfe enc (out ide the O-ring zone)

t o ve ify that machining hasnot alt er d the original mat erial pro e ties

5.1.2.2 Cel and othe ap ar atus

The c l ( e Figur 2) is comp sed of two s ainles st eel flang es embed ing the disc A v lume of

a pro imat ely 5 cm

Gas discharg es can oc ur aft er disc burs ing eithe through the lower flang e or up e flang e discharg e

port t o the atmosphe e This pe mit the ev cuation of the ins alation an a che k of the hydrog en

purity an fr edom from eithe o y g en (O

2

< 1 µl/l) or wat er v p ur (H

2

O < 3 µl/l) It also pe mit

r gulation of the g s flow an adjus ment of the pr s ur rise rat e

NOTE 1 µl/l= 1p m T e use of p m is deprecated

The seal ng devic shal be an elast ome O-ring for hel um t es ing, an for hydrog en t es ing at rat es of

mor than 1 b r/ min F or hydrog en t es ing at rat es not ex ce ding 1 b r/ min, in ium O-rings shal be

used (t o el minat e o yg en r trodifusion)

F or the flang e as embly, t en high-s r ngth st eel b lt should be used, siz M1 or eq iv lent The

tight ening t orq e shal be 3 Nm for elast ome O-rings an 1 0 Nm for in ium O-rings

Hydrogen an helum shal be stor d in high-pr s ur containe s conne ted to the tes c ls A flow control

v alve betwe n the high-pr s ur containe an the c l shal be used to adjus the pr s ur rise rate

5.1.2.3 Test pr oc ed r e

F or a satis act ory out come of the t es pe formanc s, o e ations in the folowing seq enc s shal be

car ied out

— Ev cuation of the c l b pumping t o el minat e any trac s of air or mois ur a sorbed b the wal s

Purging with the g s t o be used, folowed b v cu m pumping, can also be used t o impro e the

cleaning eff iciency

— Che k the purity of the g s flowing out of the c l befor t es ing t o ensur a senc of trac of air or

mois ur a sorbed b the walsan theg s spe if ication has be n met

— Adjus ment of the g s flow t o achieve the a pro riat e pr s ur rise rat e ( if ne es ary)

— Isolation of the c l (at the s art of pr s ur rise)

on the u per side

NOTE T e dis is lo ded with Δ = P

2– P

2

Figure 1 — C mpensating pres ure dis test principle

The rat e of pr s ur rise shal be r gular an kept as cons ant as p s ible, negle ting the g s

compr s ibi ty fact or with pr s ur

To ev luat e the beha iour of st eels at pr s ur highe than 3 0 b r, eithe a thicker disc shal be used

( e 5.1.2.1) or a compensating pr s ur of ine t g s( e Figur 1) shal be introd c d pro r s ively in

the up e part of the disc c l at the same rat e an pr s ur as hydrog en (e.g up t o 40 b r) Then, the

hydrog en pr s ur is furthe inc eased as in icat ed in 5.1.1 at a cons ant rat e t o burs or t o c ack (e.g

at 7 0b r) t o ev luat e the beha iour of the st eel at a out 7 0 b r)

The ruptur pr s ur s shal be not ed from the r corded r adings at the en of the t es The pr s ur

g ug e shal be ac urat e t o ± % for the int en ed measur d ruptur pr s ur

Thet es s shal be car ied out with hydrog en (for q alty, se 5.2.2.3) an with hel um (H

2

O < 3 µl/l)for

a rang e of pr s ur rise rat es evenly dis ribut ed betwe n 0,1 b r/ min an 1 00 b r/ min Onc a rang e

of pr s ur rise rat es showing ma imum hydrog en sensitivity has be n es a lshed, thr e ad itional

t es s shal be con uct ed within this ar a, in orde t o es a l sh the minimum v lue for the ruptur

pr s ur ( e Figur 3) Six helum t es s an ninehydrog en t es s ( i.e 1 t es sin t otal) ar enough for a

thorough mat erial ev luation

5.1.3 Treatment and inter pretation of test results

5.1.3.1 Dis thicknes

Ruptur pr s ur P

rshal be sy st ematical y cor e t ed for deviation from the “ideal”v lue cor esp n ing

t o the t es of a s an ard thick es disc

The cor e t ed ruptur pr s ur , P

is themean disc thick es

5.1.3.2 Pr esentatio and interpr etatio of test results

R uptur pr s ur s, cor e t ed as indicat ed in 5.1.3.1, shal be plott ed a ains the pr s ur rise rat e

(actual ruptur pr s ur divided b the t es d ration) ex r s ed in b r/min ( e Figur 3)

F or each hydrog en t es , calculat e the ratio given in F ormula (2):

is the theor tical helum ruptur pr s ur cor esp n ing t o the same pr s ur rise rat e as

for the hydrog en t es , calculat ed b r gr s ion from the cor e t ed helum ruptur pr s ur ;

The embrit lement in ex of a mat erial is the ma imum v lue of the a o e-mentioned ratio The mat erial

shal be conside ed as suita le for compr s ed hydrog en/embrit lng g s cy lin e s if the in ex is les

than or eq al t o two

5.1.4 Faiure in c ond cting test

If it is fou d that a faiur oc ur ed d ring the cond ction of a t es (e.g ina pro riat e surfac con ition,

a normal hardnes , ir egular pr s ur rise), the t es shal ber peat ed

r

′

H2,

embrit lement in ex) an the cy lin e design drawing inclu ing the mat erial pro e ties, chemical

comp sition an heat tr atment con itions of the t est ed cy linde shal be r port ed