ISO 4802-2:2010

Glassware — Hydrolytic resistance of the interior surfaces of glass containers — Part 2: Determination by flame spectrometry and classification

ISO 4802‑2:2010 specifies methods for determining the hydrolytic resistance of the interior surfaces of glass containers when subjected to attack by water at (121 ± 1) °C for (60 ± 1) min. The resistance is measured by determining the amount of sodium and other alkali metal or alkaline earth oxides in the extraction solution using flame atomic emission or absorption spectrometry (flame spectrometry). ISO 4802‑2:2010 also specifies 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. The test method specified in ISO 4802‑2:2010 might not be applicable to containers whose surfaces have been treated with silicon (e.g. containers that are ready for direct filling).

Verrerie — Résistance hydrolytique des surfaces internes des récipients en verre — Partie 2: Détermination par spectrométrie de flamme et classification

General Information

• Status: Withdrawn
• Publication Date: 23-Mar-2010
• Withdrawal Date: 23-Mar-2010
• ICS: 71.040.20 - Laboratory ware and related apparatus
• Technical Committee: ISO/TC 76 - Transfusion, infusion and injection, and blood processing equipment for medical and pharmaceutical use
• Drafting Committee: ISO/TC 76 - Transfusion, infusion and injection, and blood processing equipment for medical and pharmaceutical use
• Current Stage: 9599 - Withdrawal of International Standard
• Completion Date: 13-Jun-2016

Relations

• Revised: ISO 4802-2:2016 - Glassware — Hydrolytic resistance of the interior surfaces of glass containers — Part 2: Determination by flame spectrometry and classification
• Effective Date: 01-Nov-2014
• Revises: ISO 4802-2:1988 - Glassware — Hydrolytic resistance of the interior surfaces of glass containers — Part 2: Determination by flame spectrometry and classification
• Effective Date: 15-Apr-2008
• Revised: SIST ISO 4802-2:1995 - Glassware -- Hydrolytic resistance of the interior surfaces of glass containers -- Part 2: Determination by flame spectrometry and classification
• Effective Date: 12-May-2008

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 4802-2
Second edition
2010-04-01


Glassware — Hydrolytic resistance of the
interior surfaces of glass containers —
Part 2:
Determination by flame spectrometry and
classification
Verrerie — Résistance hydrolytique des surfaces internes des
récipients en verre —
Partie 2: Détermination par spectrométrie de flamme et classification





Reference number
ISO 4802-2:2010(E)
©
ISO 2010

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ISO 4802-2:2010(E)
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ii © ISO 2010 – All rights reserved

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ISO 4802-2:2010(E)
Contents Page
Foreword .iv
Introduction.v
1 Scope.1
2 Normative references.1
3 Terms and definitions .2
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
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 Testing to determine whether the containers have been surface-treated.10
9 Expression of results.10
9.1 Calculation .10
9.2 Classification .11
9.3 Distinction between containers of hydrolytic resistance container class HC 1 and
F
hydrolytic resistance container class HC 2 .11
F
9.4 Designation .11
10 Test report.12
11 Reproducibility .12
Bibliography.13

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ISO 4802-2:2010(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
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.
ISO 4802-2 was prepared by Technical Committee ISO/TC 76, Transfusion, infusion and injection equipment
for medical and pharmaceutical use.
This second edition cancels and replaces the first edition (ISO 4802-2:1988), which has been technically
revised.
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
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ISO 4802-2:2010(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.
This part of ISO 4802 contains a classification which is related to but not equivalent to the classification set up
in ISO 4802-1 for the titration method.

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INTERNATIONAL STANDARD ISO 4802-2:2010(E)

Glassware — Hydrolytic resistance of the interior surfaces of
glass containers —
Part 2:
Determination by flame spectrometry and classification
1 Scope
This part of ISO 4802 specifies:
a) methods for determining the hydrolytic resistance of the interior surfaces of glass containers when
subjected to attack by water at (121 ± 1) °C for (60 ± 1) min. The resistance is measured by determining
the amount of sodium and other alkali metal or alkaline earth oxides in the extraction solution using flame
atomic emission or absorption spectrometry (flame spectrometry);
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.
The test method specified in this part of ISO 4802 might not be applicable to containers whose surfaces have
been treated with silicon (e.g. containers that are ready for direct filling).
2 Normative references
The following referenced documents are indispensable for the application of this document. 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 719, Glass — Hydrolytic resistance of glass grains at 98 °C — Method of test and classification
ISO 720, Glass — Hydrolytic resistance of glass grains at 121 °C — Method of test and classification
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 3819, Laboratory glassware — Beakers
ISO 9187-1, Injection equipment for medical use — Part 1: Ampoules for injectables
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ISO 4802-2:2010(E)
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 Ampoules are thin-walled and have a capacity normally up to 30 ml. They are intended to be closed, after
filling, by flame sealing.
3.2
bottle
flat-bottomed container, made from moulded glass
NOTE Bottles are normally thick-walled and have a capacity usually of more than 50 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 These containers are made from borosilicate or soda-lime-silica glass.
3.5
filling volume
the defined volume of water to fill the test specimen
NOTE 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 Borosilicate glass contains a mass fraction of boric oxide between 5 % and 13 %. This glass type may also
contain aluminium oxide and/or alkaline earth oxides.
NOTE 2 Neutral glass is a borosilicate glass having a very high hydrolytic resistance and a high thermal shock
resistance. When tested according to 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.
F
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 Containers made from this glass will have a moderate hydrolytic resistance due to the chemical composition of
the glass, and comply with hydrolytic resistance container class HC 3.
F
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ISO 4802-2:2010(E)

a)  Example of a glass cylinder for pen-injectors b)  Example of an injection vial made of glass
(see ISO 13926-1) tubing (see ISO 8362-1)

c)  Example of a glass barrel d)  Example of a stem cut ampoule with
(see ISO 11040-4) constriction (see ISO 9187-1)
Figure 1 — Examples of containers
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 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 are rinsed before
F F
use.
3.9
vial
small, flat-bottomed container, made from tubing or from moulded glass
NOTE 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.
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ISO 4802-2:2010(E)
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 flame
spectrometric analysis of the extraction solutions.
5 Reagents
During the test, unless otherwise stated, use only reagents of recognised analytical grade.
5.1 Test water, complying with the requirements specified in ISO 3696 for grade 2 water or better.
5.2 Hydrochloric acid, solution, c(HCl) ≈ 2 mol/l.
5.3 Hydrochloric acid, solution, c(HCl) ≈ 6 mol/l (≈ 1 + 1).
5.4 Hydrofluoric acid, c(HF) ≈ 22 mol/l (i.e. ≈ 400 g HF/l solution).
5.5 Distilled water or water of equivalent purity (grade 3 water complying with the requirements specified
in ISO 3696).
5.6 Spectrochemical buffer solution (caesium chloride solution, CsCl).
Dissolve 80 g of caesium chloride in approximately 300 ml of test water (5.1), add 10 ml of hydrochloric acid
(5.3) and transfer to a 1 000 ml volumetric flask (6.3). Dilute to the mark with the test water (5.1) and mix.
5.7 Stock solutions.
5.7.1 Dry sodium chloride, potassium chloride and calcium carbonate at (110 ± 5) °C for 2 h. Prepare
aqueous stock solutions, using the test water (5.1), directly from the chlorides and from the calcium carbonate,
after dissolving in the minimum amount of hydrochloric acid so that all solutions have concentrations of
1 mg/ml, calculated as sodium oxide, potassium oxide and calcium oxide.
5.7.2 Commercially available standard solutions may also be used.
5.8 Standard solutions.
5.8.1 Prepare standard solutions by diluting the stock solutions (5.7) with the test water (5.1) to obtain
concentrations suitable for establishing the reference solutions in an appropriate manner, e.g. with
concentrations of 20 µg/ml of sodium oxide, potassium oxide and calcium oxide.
5.8.2 Commercially available standard solutions may also be used.
5.9 Reference solutions.
The reference solutions for establishing the calibration graph (set of calibration solutions) shall be prepared by
diluting suitable concentrated standard solutions (5.8) with the test water (5.1). They should normally cover
the optimum working ranges of the specific elements according to the instrument used for the measurement.
Typical concentration ranges of the reference solutions are
⎯ for determination by flame atomic emission spectroscopy (FAES) of sodium oxide and potassium oxide:
up to 10 µg/ml;
⎯ for determination by flame atomic absorption spectrometry (FAAS) of sodium oxide and potassium oxide:
up to 3 µg/ml;
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ISO 4802-2:2010(E)
⎯ for determination by flame atomic absorption spectrometry (FAAS) of calcium oxide: up to 7 µg/ml.
For the measurement of containers of hydrolytic resistance container classes HC 1, HC 2 or HC B
F F F
(borosilicate or highly resistant glasses), the reference solutions shall be used without addition of the
spectrochemical buffer solution (5.6).
Nevertheless, when the test is run for arbitration purposes it is recommended that the spectrochemical buffer
solution also be added to these container classes.
For the measurement of containers of hydrolytic resistance container classes HC 3 or HC D (soda-lime-
F F
silica glasses), the reference solutions shall contain a volume fraction of 5 % of the spectrochemical buffer
solution (5.6).
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.
6.2 Burettes, having a suitable capacity according to the analytical procedure to be used and complying
with the requirements specified for class A burettes in ISO 385 and made of glass of hydrolytic resistance
1)
grain class HGA 1 as specified in ISO 720 or ISO 719.
6.3 One-mark volumetric flasks, having a capacity of 1 000 ml and complying with the requirements
specified for class A one-mark volumetric flasks in ISO 1042.
6.4 Water bath, capable of being heated to approximately 80 °C.
6.5 Flame atomic absorption (FAAS) or flame atomic emission (FAES) instrument.
FAAS instruments shall be equipped with line sources for sodium, potassium and calcium; they shall be
equipped with air/propane or air/acetylene gas supplies and burners for measuring sodium and potassium,
and with a nitrous oxide/acetylene gas supply and burner for measuring calcium.
FAES instruments shall be equipped with air/propane or air/acetylene gas supplies and burners for measuring
sodium and potassium.
6.6 Beakers, having a suitable capacity and complying with the requirements specified in ISO 3819.
Before use, each new beaker shall be pretreated by subjecting it to the autoclaving conditions described in 8.3.

1) Glass of hydrolytic resistance grain class ISO 719-HGB 1 adequately meets the requirements of class HGA 1
specified in ISO 720.
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ISO 4802-2:2010(E)
7 Sample preparation
7.1 Sample size
For each container capacity to be tested, the number of containers to be measured separately is specified in
Table 1.
Table 1 — Number of containers for the determination of the hydrolytic resistance
by flame spectrometry methods
Capacit
...