SIST ISO 4802-1:2018
Glassware -- Hydrolytic resistance of the interior surfaces of glass containers -- Part 1: Determination by titration method and classification
Glassware -- Hydrolytic resistance of the interior surfaces of glass containers -- Part 1: Determination by titration method and classification
This part of ISO 4802 specifies:
a) a method for determining the hydrolytic resistance of the interior surfaces of glass containers
when subjected to attack by water at 121 °C ± 1 °C for 60 min ± 1 min. The resistance is measured
by titration of a known aliquot portion of the extraction solution produced with hydrochloric acid
solution, in which case the resistance is inversely proportional to the volume of acid required;
b) a classification of glass containers according to the hydrolytic resistance of the interior surfaces
determined by the methods specified in this part of ISO 4802.
Verrerie -- Résistance hydrolytique des surfaces internes des récipients en verre -- Partie 1: Détermination par analyse titrimétrique et classification
Steklovina - Hidrolitska odpornost notranjih površin steklenih posod - 1. del: Določanje s titracijsko metodo in klasifikacija
Ta del standarda ISO 4802 določa:
a) metodo za določanje hidrolitske odpornosti notranjih površin steklenih posod, ki so izpostavljene vodi s temperaturo 121 °C ± 1 °C za 60 minut ± 1 minuta. Odpornost se meri s titracijo znanega alikvotnega deleža ekstrakcijske raztopine, pridobljene z raztopino klorovodikove kisline; v tem primeru je odpornost obratno sorazmerna s prostornino potrebne kisline;
b) klasifikacijo steklenih posod glede na hidrolitsko odpornost notranjih površin, ki je določena z metodami, opredeljenimi v tem delu standarda ISO 4802.
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INTERNATIONAL ISO
STANDARD 4802-1
Third edition
2016-06-15
Glassware — Hydrolytic resistance
of the interior surfaces of glass
containers —
Part 1:
Determination by titration method
and classification
Verrerie — Résistance hydrolytique des surfaces internes des
récipients en verre —
Partie 1: Détermination par analyse titrimétrique et classification
Reference number
ISO 4802-1:2016(E)
©
ISO 2016
---------------------- Page: 1 ----------------------
ISO 4802-1:2016(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2016, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 4802-1:2016(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 4
5 Reagents . 4
6 Apparatus . 5
7 Sample preparation . 6
7.1 Sample size . 6
7.2 Determination of the filling volume . 6
7.2.1 Flat-bottomed containers ≤20 mm outer flange diameter (except
ampoules, syringes and cartridges) . 6
7.2.2 Flat-bottomed containers >20 mm outer flange diameter . 6
7.2.3 Round-bottomed containers. 7
7.2.4 Lipped containers . 7
7.2.5 Ampoules . 7
7.2.6 Syringes and cartridges . 7
8 Procedure. 8
8.1 General . 8
8.2 Cleaning of samples . 8
8.3 Filling and heating . 8
8.4 Analysis of the extraction solutions . 9
8.5 Test to determine whether the containers have been surface treated .10
9 Expression of results .10
9.1 Determination .10
9.2 Classification .10
9.3 Distinction between containers of hydrolytic resistance container class HC 1 and
T
hydrolytic resistance container class HC 2 .10
T
9.4 Designation .11
10 Test report .11
11 Reproducibility .12
Bibliography .13
© ISO 2016 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 4802-1:2016(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment,
as well as information about ISO’s adherence to the World Trade Organization (WTO) principles in the
Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html.
The committee responsible for this document is ISO/TC 76, Transfusion, infusion and injection, and blood
processing equipment for medical and pharmaceutical use.
This third edition cancels and replaces the second edition (ISO 4802-1:2010), which has been technically
revised in particular by amending
— the subclauses on water (test water and purified water),
— the test procedure, and
— the subclause on autoclave and steam sterilizer respectively.
ISO 4802 consists of the following parts, under the general title Glassware — Hydrolytic resistance of the
interior surfaces of glass containers:
— Part 1: Determination by titration method and classification
— Part 2: Determination by flame spectrometry and classification
iv © ISO 2016 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 4802-1:2016(E)
Introduction
This part of ISO 4802 is largely based on a method of test approved by the International Commission
on Glass (ICG), Technical Committee 2, Chemical Durability and Analysis, for measuring the hydrolytic
resistance of the interior surfaces of glass containers.
The European Pharmacopoeia Commission has adopted the principle of the determination by titration
and has set up a classification for glass containers for injectable preparations which is now included in
this part of ISO 4802. In addition, this part of ISO 4802 contains a classification of containers other than
for injectable preparations.
According to many results of international interlaboratory tests, this part of ISO 4802 specifies the test
conditions in more detail than the European Pharmacopoeia in order to increase the reproducibility of
the test results. In particular, the autoclaving cycle is described in detail.
© ISO 2016 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 4802-1:2016(E)
Glassware — Hydrolytic resistance of the interior surfaces
of glass containers —
Part 1:
Determination by titration method and classification
1 Scope
This part of ISO 4802 specifies:
a) a method for determining the hydrolytic resistance of the interior surfaces of glass containers
when subjected to attack by water at 121 °C ± 1 °C for 60 min ± 1 min. The resistance is measured
by titration of a known aliquot portion of the extraction solution produced with hydrochloric acid
solution, in which case the resistance is inversely proportional to the volume of acid required;
b) a classification of glass containers according to the hydrolytic resistance of the interior surfaces
determined by the methods specified in this part of ISO 4802.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 385, Laboratory glassware — Burettes
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 719, Glass — Hydrolytic resistance of glass grains at 98 degrees C — Method of test and classification
ISO 720, Glass — Hydrolytic resistance of glass grains at 121 degrees C — Method of test and classification
ISO 1773, Laboratory glassware — Narrow-necked boiling flasks
ISO 3819, Laboratory glassware — Beakers
ISO 9187-1, Injection equipment for medical use — Part 1: Ampoules for injectables
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
ampoule
small, normally flat-bottomed container having stems in many different forms
Note 1 to entry: Ampoules are usually thin-walled and have a capacity normally up to 30 ml. They are intended to
be closed, after filling, by flame sealing.
© ISO 2016 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO 4802-1:2016(E)
3.2
bottle
flat-bottomed container, made from moulded glass
Note 1 to entry: Bottles are normally thick-walled and have a capacity usually of more than 5 ml. They may be
of circular or other geometric cross-section. Bottles are sealed with a closure made from a material other than
glass, and not by flame-sealing.
3.3
brimful capacity
volume of water required to fill a container, placed on a flat, horizontal surface
3.4
container
article made from glass to be used as primary packaging material intended to come into direct contact
with the pharmaceutical preparations
EXAMPLE Bottles, vials, syringes, ampoules and cartridges. See also Figure 1.
Note 1 to entry: These containers are made from borosilicate or soda-lime-silica glass.
3.5
filling volume
defined volume of water to fill the test specimen
Note 1 to entry: For the determination of the filling volume, see 7.2. The filling volume is a test-specific quantity that
is used to compare container sets from different sources or lots. It has no relation to the nominal product volume.
3.6
borosilicate glass
silicate glass having a very high hydrolytic resistance due to its composition, containing significant
amounts of boric oxide
Note 1 to entry: Borosilicate glass contains a mass fraction of boric oxide usually between 5 % and 13 %. This
glass type can also contain aluminium oxide and/or alkaline earth oxides.
Note 2 to entry: Neutral glass is a borosilicate glass having a very high hydrolytic resistance and a high thermal
shock resistance. When tested in accordance with ISO 720, it meets the requirements of class HGA 1. Containers
properly made from this glass comply with hydrolytic resistance container class HC 1 of this part of ISO 4802.
T
3.7
soda-lime-silica glass
silicate glass containing a mass fraction up to approximately 15 % of alkali metal oxides – mainly
sodium oxide – and a mass fraction up to about 15 % of alkaline earth oxides, mainly calcium oxide
Note 1 to entry: Containers made from this glass have a moderate hydrolytic resistance due to the chemical
composition of the glass, and comply with hydrolytic resistance container class HC 3.
T
2 © ISO 2016 – All rights reserved
---------------------- Page: 7 ----------------------
ISO 4802-1:2016(E)
a) Example of a glass cylinder for pen–injectors b) Example of an injection vial made of glass tubing
(see ISO 13926-1) (see ISO 8362-1)
c) Example of a glass barrel d) Example of a stem cut ampoule with constriction
(see ISO 11040-4) (see ISO 9187-1)
Figure 1 — Examples of containers
© ISO 2016 – All rights reserved 3
---------------------- Page: 8 ----------------------
ISO 4802-1:2016(E)
3.8
surface treatment
treatment of the internal surface of glass containers with reagents in order to achieve a de-alkalized
surface and to produce a significantly lower release of alkali metal ions (and alkali earth metal ions)
Note 1 to entry: Surface treatment is used, for example, in order to change a soda-lime-silica glass container of
hydrolytic resistance class HC 3 to a container of hydrolytic resistance class HC 2 container. Treated containers
T T
are rinsed before use.
3.9
vial
small, flat-bottomed container, made from tubing or from moulded glass
Note 1 to entry: Vials are normally thick-walled and have a capacity up to 100 ml. They are normally sealed with
a closure made from a material other than glass, and not by flame-sealing.
4 Principle
This method of test is a surface test applied to glass containers as produced and/or as delivered.
The containers to be tested are filled with specified water to a specified capacity. They are loosely
capped and then heated under specified conditions. The degree of the hydrolytic attack is measured by
titration of the extraction solutions.
5 Reagents
During the test, unless otherwise stated, use only reagents of recognized analytical grade.
5.1 Test water, to be prepared as follows:
Prepare the test water from distilled water (5.6) by multiple distillations. Remove the carbon dioxide by
boiling for at least 15 min before use in a boiling flask (6.3) of fused silica or borosilicate glass and cool.
NOTE 1 Any other suitable method can be used.
When tested immediately before use, water prepared as described above shall produce an orange-
red (not violet-red or yellow) colour corresponding to the neutral point of methyl red indicator of
pH 5,5 ± 0,1 when 0,05 ml of methyl red indicator solution (5.5) is added to 50 ml of the water to be
examined.
This water may also be used as the reference solution (see 8.4).
The conductivity of the water shall not exceed 1 µS/cm, determined at 25 °C by an in-line
conductivity meter.
[12]
NOTE 2 This description is based on the European Pharmacopoeia 3.2.1 . In the European Pharmacopoeia,
water prepared as described above is designated water R1.
[2]
NOTE 3 Water of Grade 2 according to ISO 3696 is suitable for this test.
5.2 Hydrochloric acid, standard volumetric solution, c(HCl) = 0,01 mol/l.
5.3 Hydrochloric acid, solution, c(HCl) ≈ 2 mol/l.
5.4 Hydrofluoric acid, c(HF) ≈ 22 mol/l (i.e. ≈400 g HF/l solution).
CAUTION — Hydrofluoric acid is very toxic and highly corrosive. Consider material safety
data sheet!
4 © ISO 2016 – All rights reserved
---------------------- Page: 9 ----------------------
ISO 4802-1:2016(E)
5.5 Methyl red, indicator solution.
Dissolve 25 mg of the sodium salt of methyl red (C H N NaO ) in 100 ml of the test water (5.1).
15 14 3 2
5.6 Purified water, prepared by distillation, by ion exchange, by reverse osmosis or by any other
suitable method from water having drinking water quality.
NOTE 1 See national or regional regulation on water intended for human consumption.
[2]
NOTE 2 Water that corresponds to Grade 3 according to ISO 3696 is suitable.
[12]
NOTE 3 In the European Pharmacopoeia 3.2.1 , water as described above is designated water R.
6 Apparatus
Ordinary laboratory apparatus and those specified in 6.1 to 6.6.
6.1 Autoclave or steam sterilizer, capable of withstanding a pressure of at least 250 kPa (2,5 bar)
and of carrying out the heating cycle specified in 8.3. It shall be capable of maintaining a temperature of
(121 ± 1) °C, equipped with a calibrated thermometer or a calibrated thermocouple recorder, a pressure
gauge and a vent-cock.
When necessary and appropriate, the autoclave vessel and ancillary equipment shall be thoroughly
cleaned before use using the test water (5.1) in order to avoid contamination that can influence the test
results.
Most recent autoclave models are not provided with a vent cock that can be operated manually. The
operator is referred to the user instructions and/or technical description provided by the manufacturer
of the aut
...
SLOVENSKI STANDARD
SIST ISO 4802-1:2018
01-september-2018
1DGRPHãþD
SIST ISO 4802-1:1995
6WHNORYLQD+LGUROLWVNDRGSRUQRVWQRWUDQMLKSRYUãLQVWHNOHQLKSRVRGGHO
'RORþDQMHVWLWUDFLMVNRPHWRGRLQNODVLILNDFLMD
Glassware -- Hydrolytic resistance of the interior surfaces of glass containers -- Part 1:
Determination by titration method and classification
Verrerie -- Résistance hydrolytique des surfaces internes des récipients en verre -- Partie
1: Détermination par analyse titrimétrique et classification
Ta slovenski standard je istoveten z: ISO 4802-1:2016
ICS:
71.040.20 Laboratorijska posoda in Laboratory ware and related
aparati apparatus
SIST ISO 4802-1:2018 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST ISO 4802-1:2018
---------------------- Page: 2 ----------------------
SIST ISO 4802-1:2018
INTERNATIONAL ISO
STANDARD 4802-1
Third edition
2016-06-15
Glassware — Hydrolytic resistance
of the interior surfaces of glass
containers —
Part 1:
Determination by titration method
and classification
Verrerie — Résistance hydrolytique des surfaces internes des
récipients en verre —
Partie 1: Détermination par analyse titrimétrique et classification
Reference number
ISO 4802-1:2016(E)
©
ISO 2016
---------------------- Page: 3 ----------------------
SIST ISO 4802-1:2018
ISO 4802-1:2016(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2016, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 4802-1:2018
ISO 4802-1:2016(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 4
5 Reagents . 4
6 Apparatus . 5
7 Sample preparation . 6
7.1 Sample size . 6
7.2 Determination of the filling volume . 6
7.2.1 Flat-bottomed containers ≤20 mm outer flange diameter (except
ampoules, syringes and cartridges) . 6
7.2.2 Flat-bottomed containers >20 mm outer flange diameter . 6
7.2.3 Round-bottomed containers. 7
7.2.4 Lipped containers . 7
7.2.5 Ampoules . 7
7.2.6 Syringes and cartridges . 7
8 Procedure. 8
8.1 General . 8
8.2 Cleaning of samples . 8
8.3 Filling and heating . 8
8.4 Analysis of the extraction solutions . 9
8.5 Test to determine whether the containers have been surface treated .10
9 Expression of results .10
9.1 Determination .10
9.2 Classification .10
9.3 Distinction between containers of hydrolytic resistance container class HC 1 and
T
hydrolytic resistance container class HC 2 .10
T
9.4 Designation .11
10 Test report .11
11 Reproducibility .12
Bibliography .13
© ISO 2016 – All rights reserved iii
---------------------- Page: 5 ----------------------
SIST ISO 4802-1:2018
ISO 4802-1:2016(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment,
as well as information about ISO’s adherence to the World Trade Organization (WTO) principles in the
Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html.
The committee responsible for this document is ISO/TC 76, Transfusion, infusion and injection, and blood
processing equipment for medical and pharmaceutical use.
This third edition cancels and replaces the second edition (ISO 4802-1:2010), which has been technically
revised in particular by amending
— the subclauses on water (test water and purified water),
— the test procedure, and
— the subclause on autoclave and steam sterilizer respectively.
ISO 4802 consists of the following parts, under the general title Glassware — Hydrolytic resistance of the
interior surfaces of glass containers:
— Part 1: Determination by titration method and classification
— Part 2: Determination by flame spectrometry and classification
iv © ISO 2016 – All rights reserved
---------------------- Page: 6 ----------------------
SIST ISO 4802-1:2018
ISO 4802-1:2016(E)
Introduction
This part of ISO 4802 is largely based on a method of test approved by the International Commission
on Glass (ICG), Technical Committee 2, Chemical Durability and Analysis, for measuring the hydrolytic
resistance of the interior surfaces of glass containers.
The European Pharmacopoeia Commission has adopted the principle of the determination by titration
and has set up a classification for glass containers for injectable preparations which is now included in
this part of ISO 4802. In addition, this part of ISO 4802 contains a classification of containers other than
for injectable preparations.
According to many results of international interlaboratory tests, this part of ISO 4802 specifies the test
conditions in more detail than the European Pharmacopoeia in order to increase the reproducibility of
the test results. In particular, the autoclaving cycle is described in detail.
© ISO 2016 – All rights reserved v
---------------------- Page: 7 ----------------------
SIST ISO 4802-1:2018
---------------------- Page: 8 ----------------------
SIST ISO 4802-1:2018
INTERNATIONAL STANDARD ISO 4802-1:2016(E)
Glassware — Hydrolytic resistance of the interior surfaces
of glass containers —
Part 1:
Determination by titration method and classification
1 Scope
This part of ISO 4802 specifies:
a) a method for determining the hydrolytic resistance of the interior surfaces of glass containers
when subjected to attack by water at 121 °C ± 1 °C for 60 min ± 1 min. The resistance is measured
by titration of a known aliquot portion of the extraction solution produced with hydrochloric acid
solution, in which case the resistance is inversely proportional to the volume of acid required;
b) a classification of glass containers according to the hydrolytic resistance of the interior surfaces
determined by the methods specified in this part of ISO 4802.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 385, Laboratory glassware — Burettes
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 719, Glass — Hydrolytic resistance of glass grains at 98 degrees C — Method of test and classification
ISO 720, Glass — Hydrolytic resistance of glass grains at 121 degrees C — Method of test and classification
ISO 1773, Laboratory glassware — Narrow-necked boiling flasks
ISO 3819, Laboratory glassware — Beakers
ISO 9187-1, Injection equipment for medical use — Part 1: Ampoules for injectables
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
ampoule
small, normally flat-bottomed container having stems in many different forms
Note 1 to entry: Ampoules are usually thin-walled and have a capacity normally up to 30 ml. They are intended to
be closed, after filling, by flame sealing.
© ISO 2016 – All rights reserved 1
---------------------- Page: 9 ----------------------
SIST ISO 4802-1:2018
ISO 4802-1:2016(E)
3.2
bottle
flat-bottomed container, made from moulded glass
Note 1 to entry: Bottles are normally thick-walled and have a capacity usually of more than 5 ml. They may be
of circular or other geometric cross-section. Bottles are sealed with a closure made from a material other than
glass, and not by flame-sealing.
3.3
brimful capacity
volume of water required to fill a container, placed on a flat, horizontal surface
3.4
container
article made from glass to be used as primary packaging material intended to come into direct contact
with the pharmaceutical preparations
EXAMPLE Bottles, vials, syringes, ampoules and cartridges. See also Figure 1.
Note 1 to entry: These containers are made from borosilicate or soda-lime-silica glass.
3.5
filling volume
defined volume of water to fill the test specimen
Note 1 to entry: For the determination of the filling volume, see 7.2. The filling volume is a test-specific quantity that
is used to compare container sets from different sources or lots. It has no relation to the nominal product volume.
3.6
borosilicate glass
silicate glass having a very high hydrolytic resistance due to its composition, containing significant
amounts of boric oxide
Note 1 to entry: Borosilicate glass contains a mass fraction of boric oxide usually between 5 % and 13 %. This
glass type can also contain aluminium oxide and/or alkaline earth oxides.
Note 2 to entry: Neutral glass is a borosilicate glass having a very high hydrolytic resistance and a high thermal
shock resistance. When tested in accordance with ISO 720, it meets the requirements of class HGA 1. Containers
properly made from this glass comply with hydrolytic resistance container class HC 1 of this part of ISO 4802.
T
3.7
soda-lime-silica glass
silicate glass containing a mass fraction up to approximately 15 % of alkali metal oxides – mainly
sodium oxide – and a mass fraction up to about 15 % of alkaline earth oxides, mainly calcium oxide
Note 1 to entry: Containers made from this glass have a moderate hydrolytic resistance due to the chemical
composition of the glass, and comply with hydrolytic resistance container class HC 3.
T
2 © ISO 2016 – All rights reserved
---------------------- Page: 10 ----------------------
SIST ISO 4802-1:2018
ISO 4802-1:2016(E)
a) Example of a glass cylinder for pen–injectors b) Example of an injection vial made of glass tubing
(see ISO 13926-1) (see ISO 8362-1)
c) Example of a glass barrel d) Example of a stem cut ampoule with constriction
(see ISO 11040-4) (see ISO 9187-1)
Figure 1 — Examples of containers
© ISO 2016 – All rights reserved 3
---------------------- Page: 11 ----------------------
SIST ISO 4802-1:2018
ISO 4802-1:2016(E)
3.8
surface treatment
treatment of the internal surface of glass containers with reagents in order to achieve a de-alkalized
surface and to produce a significantly lower release of alkali metal ions (and alkali earth metal ions)
Note 1 to entry: Surface treatment is used, for example, in order to change a soda-lime-silica glass container of
hydrolytic resistance class HC 3 to a container of hydrolytic resistance class HC 2 container. Treated containers
T T
are rinsed before use.
3.9
vial
small, flat-bottomed container, made from tubing or from moulded glass
Note 1 to entry: Vials are normally thick-walled and have a capacity up to 100 ml. They are normally sealed with
a closure made from a material other than glass, and not by flame-sealing.
4 Principle
This method of test is a surface test applied to glass containers as produced and/or as delivered.
The containers to be tested are filled with specified water to a specified capacity. They are loosely
capped and then heated under specified conditions. The degree of the hydrolytic attack is measured by
titration of the extraction solutions.
5 Reagents
During the test, unless otherwise stated, use only reagents of recognized analytical grade.
5.1 Test water, to be prepared as follows:
Prepare the test water from distilled water (5.6) by multiple distillations. Remove the carbon dioxide by
boiling for at least 15 min before use in a boiling flask (6.3) of fused silica or borosilicate glass and cool.
NOTE 1 Any other suitable method can be used.
When tested immediately before use, water prepared as described above shall produce an orange-
red (not violet-red or yellow) colour corresponding to the neutral point of methyl red indicator of
pH 5,5 ± 0,1 when 0,05 ml of methyl red indicator solution (5.5) is added to 50 ml of the water to be
examined.
This water may also be used as the reference solution (see 8.4).
The conductivity of the water shall not exceed 1 µS/cm, determined at 25 °C by an in-line
conductivity meter.
[12]
NOTE 2 This description is based on the European Pharmacopoeia 3.2.1 . In the European Pharmacopoeia,
water prepared as described above is designated water R1.
[2]
NOTE 3 Water of Grade 2 according to ISO 3696 is suitable for this test.
5.2 Hydrochloric acid, standard volumetric solution, c(HCl) = 0,01 mol/l.
5.3 Hydrochloric acid, solution, c(HCl) ≈ 2 mol/l.
5.4 Hydrofluoric acid, c(HF) ≈ 22 mol/l (i.e. ≈400 g HF/l solution).
CAUTION — Hydrofluoric acid is very toxic and highly corrosive. Consider material safety
data sheet!
4 © ISO 2016 – All rights reserved
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SIST ISO 4802-1:2018
ISO 4802-1:2016(E)
5.5 Methyl red, indicator solution.
Dissolve 25 mg of the sodium salt of methyl red (C H N NaO ) in 100 ml of the test water (5.1).
15 14 3 2
5.6 Purified water, prepared by distillation, by ion exchange, by reverse osmosis or by any other
suitable method from water having drinking water quality.
NOTE 1 See national or regional regulation on water intended for human consumption.
[2]
NOTE 2 Water that corresponds to Grade 3 according to ISO 3696 is suitable.
[12]
NOTE 3 In the European Pharmacopoeia 3.2.1 , water as described above is designated water R.
6 Apparatus
Ordinary laboratory apparatus and those specified in 6.1 to 6.6.
6.1 Autoclave or steam sterilizer, capable of withstanding a pressure of at least 250 kPa (2,5 bar)
and of carrying out the heating cycle specified in 8.3. It s
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