Tiêu chuẩn iso 04802 1 2016

© ISO 2016 Glassware — Hydrolytic resistance of the interior surfaces of glass containers — Part 1 Determination by titration method and classification Verrerie — Résistance hydrolytique des surfaces[.]

Glassware — Hydrol ytic resistanc e

Part 1:

Ve r rie — Résista c h drolytique de s surfce s inte ne s de s

récipient en ve r —

Partie 1: Déte mination p r a alyse titrimétrique et classification

T ir d edition

2 16-06-1

COPYRIGHT PROTECTED DOCUMENT

© ISO 2016, 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

the r eq eser

ISO c pyrig ht ofic

C de Blan on et 8 • C 4 1

CH-1 14 Vernier, Geneva, Sw itzerlan

Tel + 12 7 9 011

Fax 412 7 9 0 4

c pyrig ht@iso.or g

www.iso.or g

F reword i v

Introduction v

1 Sc ope 1

2 Nor mati ve r eferenc es 1

3 Terms and definitions 1

4 Principle 4

5 Re g ents 4

6 A pparatus 5

7 S mple preparatio 6

7.1 Sample siz 6

7.2 Dete mination of the fi ing v lume 6

7.2.1 Flat-b tomed containe s ≤ 0 mm oute flang ediamete (exc pt amp ules, syring esan cartridg es) 6

7.2.2 Flat-b tomed containe s > 0 mm oute flang ediamete 6

7.2.3 Rou d-b ttomed containe s 7

7.2.4 Lipped containe s 7

7.2.5 A mp ules 7

7.2.6 Syring es an cartridg es 7

8 Proc ed re .8

8.1 General 8

8.2 Cleaning of samples 8

8.3 Fi ing and heating 8

8.4 A nalysis of the extraction solutions 9

8.5 Tes to dete mine whethe the containe s ha ve be n surfac tr eated 1

9 Ex pres io of r esults 10

9.1 Dete mination 1

9.2 Clas ification 1

9.3 Dis inction betwe n containe s of hydr olytic r esistanc containe clas HC T 1 an hydr olytic r esistanc containe clas HC T 2 1

9.4 Desig nation 1

10 Test rep r t 11

11 Reproducibiity 12

Biblog raphy 13

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 ove nmental 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 t erms an ex r s ions r lated 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 this document is ISO/TC76, Tra s fus io , in us ion a d injec tion, a d blo d

proc es s in eq ipment fr medic al a d p armaceutic al us e

This third edition canc ls an r plac s the se on edition (ISO 480 -1:2 1 ), w hich has be n t ech icaly

r vised in p rticular b amen ing

— thesubclauses on wat er (t es wat er an purified wat er),

— thet es proc d r , an

— thesubclause on aut ocla e an st eam st eri iz r r spe tively

ISO 48 2 consis s of the folowing p rt , u de the g ene al title Glas swar — Hydroly tic r s i s ta c e o the

inte ior s urfc es o glas s c ontaine s:

— Part 1: Dete min tio  b titratio  meth d a d clas s ific ation

— Part 2 : Dete min tio  b  flame s pec trometry a d clas s ific atio

This p rt ofISO 48 2 is larg ely b sed on a method of t es a pro ed b the Int ernational Commis ion

on Glas (ICG), Te h ical C mmitt ee 2, Chemic al Dura i t y a d An lys i s, for measuring the hydrolytic

r sis anc of the int erior surfac s of glas containe s

The E ro ean P armaco oeia C mmis ion has ado t ed the principle of the det ermination b titration

an has set up a clas if ication for glas containe s for inje ta le pr p rations w hich is now inclu ed in

this p rt of ISO 480 In ad ition, this p rt of ISO 48 2 containsa clas if ication of containe s othe than

for inje ta le pr p rations

A ccording t o many r sult of int ernational int erla orat ory t es s, this p rt of ISO 48 2 spe if ies the t es

con itions in mor detai than the E ro ean P armaco oeia in orde t o inc ease the r prod cibi ity of

the t es r sult In p rticular, the aut ocla ing cycle is desc ibed in detai

Glassware — Hydrol ytic resistanc e ofthe interior surfac es

Part 1:

This part of ISO 480 spe ifies:

a) a method for det ermining the hydrolytic r sis anc of the int erior surfac s of glas containe s

w hen subje t ed t o at ack b wat er at 1 1 °C ± 1 °C for 6 min ± 1 min The r sis anc is measur d

b titration of a k own alq ot portion of the extraction solution prod c d with hydrochloric acid

solution, in w hich case ther sis anc is inve sely pro ortional t o the volume of acid r q ir d;

b) a clas if ication of glas containe s ac ording t o the hydrolytic r sis anc of the int erior surfac s

det ermined b the methods spe if ied in this p rt of ISO 48 2

2 Normati ve r eferences

The folowing document , in w hole or in p rt, ar normatively r fe enc d in this document an ar

in ispensa le for it a pl cation F or dat ed r fe enc s, only the edition cit ed a pl es F or u dat ed

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

ISO 3 5, L b rator y glas swar — B ur ttes

ISO 648, L b rator y glas swar — Sin le-v lume pipet es

ISO 7 9, Glas s — Hydroly tic  r s i s ta c e o glas s grains at 98 degr es C — Meth d o tes t a d clas s ific atio

ISO 7 0, Glas s — Hydroly tic r s i s ta c e o glas s grains at 121 degr es C — Meth d o tes t a d clas s ific atio

ISO 1 7 , L b ratory glas swar  — Nar ow-necked b i n  flask s

ISO 3 1 , L b rator y glas swar — B eake s

ISO 9 8 -1, Injec tion eq ipment fr medic al use — Part 1: Amp ules fr injec ta les

3 Terms and definitions

F or the purposes of this document, the folowing t ermsand definitions a ply

3.1

smal, normal y flat-bott omed containe ha ing st ems in many dife ent forms

Note 1 t o entry: Ampoules are usual y thin-wal ed an have a capacity normal y u to 3 ml They are inten ed to

b closed, afer f il ing,by flame se ling

bot le

flat-b tt omed containe , madefrom moulded glas

Not e 1 to entry: Bot les are normal y thick-waled an have a capacity usualy of more than 5 ml They may b

of cir ular or other g ometric c os -section Bot les are se led with a closure made from a material other than

glas , an not by flame-se ling

3.3

brimful capacity

v lume of wat er r q ir d t o f il a containe , plac d on a flat, horizontal surfac

3.4

co tainer

article made from glas t o be used as primary packa ing mat erial int en ed t o come int o dir ct contact

with the pharmac utical pr p rations

E AMP E Bot les,vials, syring s, ampoules an cartridg es S e also Figure 1

Not e 1t o entry: T ese container are made from b rosilicate or soda-lime-silica glas

3.5

fi lng v lume

defined v lume of wat er t o fil the t es spe imen

Not e 1t o entry : F or the det ermination of the fil ing volume, se 7.2 T e filing volume is a t est-specific q antity that

is used t o compare container ets from diferent sour es or lots It has no relation t o the nominal prod ct volume

3.6

borosi icate glas

si icat e glas ha ing a ve y high hydrolytic r sis anc d e t o it composition, containing significant

amou t of boric o ide

Not e 1 t o entry: Borosilicat e glas contains a mas fraction of b ric o ide usualy b tween 5 % an 1 % T is

glas ty e can also contain aluminium o ide an / r alkaline e rth o ides

Not e 2 t o entry: Neutral glas is a b rosilicat e glas having a very high hydrolytic resistance an a high thermal

shock resistance When t est ed in ac ordance with ISO 72 , it me ts the req irements of clas HG 1 Container

properly made from this glas comply with hydrolytic resistance container clas HC

T

1 of this part of ISO 48 2

3.7

so a- ime-si ica glas

si icat e glas containing a mas fraction up t o a pro imat ely 1 % of alkal metal o ides – mainly

sodium o ide – an a mas fraction up t o a out 1 % of alkal ne earth o ides, mainly calcium o ide

Not e 1 to entry: Container made from this glas have a moderate hydrolytic resistance d e t o the chemical

composition of the glas , an comply with hydrolytic resistance container clas HC

T

3

a) Ex mple of a glas cy lin e for pen–inje t ors

( e ISO 1 9 6-1)

b)E ample of an inje tion vial made of glas tubing

( e ISO 8 6 -1)

c) E ample of a glas b r el

( e ISO 1 0 0-4)

d)E ample of a st em cut amp ule with cons riction

( e ISO 9 87-1)

Figure 1 — Examples of container

surface tre tment

tr atment of the int ernal surfac of glas containe s with r ag ent in orde t o achieve a de-alkal z d

surfac an t o prod c a signif icantly lowe r lease of alkal metal ions (an alkal earth metal ions)

Not e 1 to entry: Surface tre tment is used, for e ample, in order t o chang a soda-lime-silica glas container of

hydrolytic resistance clas HC

T

3 t o a container of hydrolytic resistance clas HC

T

2 container Tre ted container

are rinsed b fore use

3 9

vial

smal, flat-b tt omed containe , made from tubing or from moulded glas

Not e 1t o entry: Vials are normaly thick-wal ed an have a capacity u to 1 0ml T ey are normaly se led with

a closure made from a material other than glas , an not by flame-se ling

This method of t es isa surfac t es a pled t o glas containe s as prod c d an / r as delver d

The containe s t o be t est ed ar f iled with spe if ied wat er t o a spe ified ca acity They ar lo sely

ca ped an then heat ed u de spe if ied con itions The degr e of the hydrolytic at ack is measur d b

titration of theextraction solutions

During the t es , u les othe wise s at ed, use only r ag ent of r co niz d analytical grade

5.1 Test water , to be pr ep r ed as folows:

Pr p r the t es wat er from dis i ed wat er (5.6) b multiple dis i lations Remo e the carb n dio ide b

b i ng for at leas 1 min befor use in a b i ing flask (6.3) of fused si ca or b rosi icat e glas an co l

NOTE 1 An other suita le method can b used

When t est ed immediat ely befor use, wat er pr par d as desc ibed a o e shal prod c an orang

e-r d (not violet-r d or yelow) colour cor espon ing t o the neutral p int of methy l r d indicat or of

pH 5,5 ± 0,1 w hen 0,0 ml of methy l r d in icat or solution (5.5) is ad ed t o 5 ml of the wat er t o be

ex mined

This wat er ma also be used as the r fe enc solution ( e 8.4)

The con uctivity of the wate shal not exc ed 1 µS/cm, dete mined at 25 °C b an in-l ne

con uctivity mete

NOTE 2 T is des ription is b sed on the E rope n P armacopo ia 3.2.1

[1 ]

In the E rope n P armacopo ia,

water prepared as des rib d a ove is designated wat er R 1

NOTE 3 Wat er of Grade 2ac ording to ISO 3696

[2]

is suita le for this test

5.2 Hy rochloric acid, s an ar d v lumetric solution, c (HCl) = 0,0 mol/l

5.3 Hy rochloric acid, solution, c(HCl) ≈ 2 mol/l

5.4 Hy rofluor ic acid, c(HF) ≈ 22 mol/l (i.e ≈ 0 g HF l solution)

CA UTION — Hy drofluoric acid is v ery to ic and highly cor osiv e C nsider material safety

data she t !

5.5 Methyl red, in icator solution.

Dis olve 2 mg of the sodium salt of methy l r d (C

1 H

14 N

3 NaO

2 ) in 1 0 ml of the t es wat er (5.1)

5.6 Purified water, pr ep r ed b dis i ation, b ion exchange, b r eve se osmosis or b any othe

suita le method fr om wate ha ving drinking wate q alty

NOTE 1 S e national or re ional re ulation on wat er inten ed for h man consumption

NOTE 2 Water that cor espon s t o Grade 3 ac ording to ISO 3696

[2]

is suita le

NOT 3 In the E rope n P armacopo ia 3.2.1

[1 ]

, water as des rib d a ove is designated water R

6 A pparatus

Ordinary la orat ory a p ratus an those spe if ied in 6.1 t o 6.6

6.1 Autoclave or ste m ster ilzer, ca a le of w ithstanding a pr es ur e of at leas 2 0 k a (2,5 b r)

and of car ying out the heating cycle spe ified in 8.3 It shal be ca a le of maintaining a temper atur e of

(1 1 ± 1) °C, eq ipped with a calbr ated the momete or a calbr ated the mocouple recorde , a pr es ur e

gaug e and a vent-cock

When ne es ary an a pro riat e, the aut ocla e ves el an anci lary eq ipment shal be thoroughly

cleaned befor use using the t es wat er (5.1)in orde t o a oid contamination that can influenc the t es

r sult

Mos r c nt aut ocla e models ar not pro ided with a vent cock that can be o e at ed man aly The

o e at or isr fe r d t o the use ins ructions an / r t ech ical desc iption pro ided b the man factur r

of the aut ocla e with r g rd t o the fu ctioning of the venting o e ations A time /t empe atur print out

can be used as evidenc of a pro e venting s ag e

F or a ut ocla es using a st eam g ene at or, it is not ne es ary t o hold the t empe atur at 1 0 °C for 1 min

6.2 Bur et es, ha ving a suita le ca acity of 5 ml, 2 ml, 1 ml or 2 ml, complying with the req irement

spe ified for clas A buretes in ISO 3 5 an made of glas of hydr olytic r esis anc g rain clas HGA 1 as

spe ified in ISO 7 9 or ISO 72

1)

The ca acity of the bur tt es shal be chosen ac ording t o the ex e t ed consumption of hydrochloric

acid (5.2)

6.3 C nical flasks, ha ving a ca acity of 1 0 ml an 25 ml an complying with the r eq ir ement of

ISO 1 7

Befor it firs use, each flask shal be pr tr at ed b fil ng with purif ied wat er (5.6) an a ut ocla ing at

1 1 °C for at leas 1 h ( e 8.3)

IMPORT ANT — If it is intended to use these flasks for other purposes, before being re-used in

ac ordance with this part of ISO 4802, the flasks shal be properly cle ned (e.g by tre tment

with hy rochloric acid and/or by autoclave cle ning)

6.4 Pipet es, ha ving a suitable ca acity an complying with the r eq ir ement spe ified for clas A

pipetes desc ibed in ISO 648