1、February 2017 English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 11.100.99; 71.040.20!%_z“260879
2、8www.din.deDIN ISO 4802-2Glassware Hydrolytic resistance of the interior surfaces of glass containers Part 2: Determination by flame spectrometry and classification (ISO 48022:2016),English translation of DIN ISO 4802-2:2017-02Glasartikel Wasserbestndigkeit der inneren Oberflche von Glasbehltern Tei
3、l 2: Bestimmung durch Flammenspektrometrie und Klasseneinteilung (ISO 48022:2016),Englische bersetzung von DIN ISO 4802-2:2017-02Verrerie Rsistance hydrolytique des surfaces internes des rcipients en verre Partie 2: Dtermination par spectromtrie de flamme et classification (ISO 48022:2016),Traductio
4、n anglaise de DIN ISO 4802-2:2017-02SupersedesDIN ISO 48022:201212www.beuth.deDocument comprises 19 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.02.17 A comma is used as the decimal marker. Contents Page Introduction 51 Scop
5、e . 62 Normative references 63 Terms and definitions . 64 Principle 95 Reagents 96 Apparatus 117 Sample preparation 117.1 Sample size 117.2 Determination of the filling volume . 127.2.1 Flat-bottomed containers 20 mm outer flange diameter (except ampoules, syringes and cartridges) . 127.2.2 Flat-bot
6、tomed containers 20 mm outer flange diameter . 127.2.3 Round-bottomed containers. 127.2.4 Lipped containers 137.2.5 Ampoules . 137.2.6 Syringes and cartridges 138 Procedure 138.1 General 138.2 Cleaning of samples . 148.3 Filling and heating 148.4 Analysis of the extraction solutions . 158.4.1 Contai
7、ners of hydrolytic resistance container classes HCF1, HCF2 and HC B or those known to be made from borosilicate glassF158.4.2 Containers of hydrolytic resistance container classes HCF3 and HCFD, or those known to be made from soda-lime-silica glass .158.5 Testing to determine whether the containers
8、have been surface-treated .169 Expression of results .169.1 Determination 169.2 Classification 179.3 Distinction between containers of hydrolytic resistance container class HCF1 and hydrolytic resistance container class HCF2 179.4 Designation . 1710 Test report 1711 Reproducibility .18Bibliography .
9、19National foreword 3 Nationaler Annex NA (informative) Bibliography 4 2DIN ISO 4802-2:2017-02 National foreword This document (ISO 4802-2:2016) has been prepared by Technical Committee ISO/TC 76 “Transfusion, infusion and injection, and blood processing equipment for medical and pharmaceutical use”
10、 with the active participation of German experts. The responsible German body involved in its preparation was DIN-Normenausschuss Medizin (DIN Standards Committee Medicine), Working Committee NA 063-02-03 AA Verpackungssysteme fr die Befllung und Applikation von medizinischen Produkten. Attention is
11、 drawn to the possibility that some of the elements of this document may be the subject of patent rights. DIN shall not be held responsible for identifying any or all such patent rights. The DIN ISO 4802 series consists of the following parts, under the general title Glassware Hydrolytic resistance
12、of the interior surfaces of glass containers: Part 1: Determination by titration method and classification Part 2: Determination by flame spectrometry and classification The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 385 DIN EN ISO 385
13、 ISO 719 DIN ISO 719 ISO 720 DIN ISO 720 ISO 1042 DIN EN ISO 1042 ISO 3585 DIN ISO 8535 ISO 3696 DIN ISO 3696 ISO 3819 DIN EN ISO 3819 ISO 8362-1 DIN EN ISO 8362-1 ISO 8362-4 DIN EN ISO 8362-4 ISO 8536-1 DIN EN ISO 8536-1 ISO 9187-1 DIN EN ISO 9187-1 ISO 13926-1 DIN ISO 13926-1 ISO 11040-1 DIN ISO 1
14、1040-1 ISO 11040-4 DIN ISO 11040-4 ISO 11418-1 DIN ISO 11418-1 ISO 11418-4 DIN ISO 11418-4 ISO 11418-7 DIN ISO 11418-7 Amendments This standard differs from DIN ISO 4802-2:2012-12 as follows: a) subclauses on water (test water and purified water) have been revised; b) test methods have been revised;
15、 c) the subclause on autoclaves and steam sterilizers has been revised; d) the text of the standard has been editorially revised. Previous editions DIN 52339-2: 1980-12 DIN EN ISO 4802-2: 2012-12 3DIN ISO 4802-2:2017-02 National Annex NA (informative) Bibliography DIN EN ISO 385, Laboratory glasswar
16、e Burettes DIN EN ISO 1042, Laboratory glassware One-mark volumetric flasks DIN EN ISO 3819, Laboratory glassware Beakers DIN EN ISO 8362-1, Injection containers and accessories Part 1: Injection vials made of glass tubing DIN EN ISO 8362-4, Injection containers and accessories Part 4: Injection via
17、ls made of moulded glass DIN EN ISO 8536-1, Infusion equipment for medical use Part 1: Infusion glass bottles DIN EN ISO 9187-1, Injection equipment for medical use Part 1: Ampoules for injectables DIN ISO 719, Glass Hydrolytic resistance of glass grains at 98 C Method of test and classification DIN
18、 ISO 720, Glass Hydrolytic resistance of glass grains at 121 C Method of test and classification DIN ISO 3585, Borosilicate glass 3.3 Properties DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO 11040-1, Prefilled syringes Part 1: Glass cylinders for dental loc
19、al anaesthetic cartridges DIN ISO 11040-4, Prefilled syringes Part 4: Glass barrels for injectables DIN ISO 11418-1, Containers and accessories for pharmaceutical preparations Part 1: Drop-dispensing glass bottles DIN ISO 11418-4, Containers and accessories for pharmaceutical preparations Part 4: Ta
20、blet glass bottles DIN ISO 11418-7, Containers and accessories for pharmaceutical preparations Part 7: Screw-neck vials made of glass tubing for liquid dosage forms DIN ISO 13926-1, Pen systems Part 1: Glass cylinders for pen-injectors for medical use 4DIN ISO 4802-2:2017-02 IntroductionThis part of
21、 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
22、is related to but not equivalent to the classification set up in ISO 4802-1 for the titration method.5DIN ISO 4802-2:2017-02 Glassware Hydrolytic resistance of the interior surfaces of glass containers Part 2: Determination by flame spectrometry and classification1 ScopeThis part of ISO 4802 specifi
23、es: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 solutio
24、n 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
25、not be applicable to containers whose surfaces have been treated with silicon (e.g. containers that are ready for direct filling).2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated refer
26、ences, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 385, Laboratory glassware BurettesISO 719, Glass Hydrolytic resistance of glass grains at 98 degrees C Method of test and classificationISO 720, Glass H
27、ydrolytic resistance of glass grains at 121 degrees C Method of test and classificationISO 1042, Laboratory glassware One-mark volumetric flasksISO 3819, Laboratory glassware BeakersISO 9187-1, Injection equipment for medical use Part 1: Ampoules for injectables3 Terms and definitionsFor the purpose
28、s of this document, the following terms and definitions apply.3.1ampoulesmall, normally flat-bottomed container having stems in many different formsNote 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 seal
29、ing.6DIN ISO 4802-2:2017-02 3.2bottleflat-bottomed container, made from moulded glassNote 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 othe
30、r than glass, and not by flame-sealing.3.3brimful capacityvolume of water required to fill a container, placed on a flat, horizontal surface3.4containerarticle made from glass to be used as primary packaging material intended to come into direct contact with the pharmaceutical preparationsEXAMPLE Bo
31、ttles, vials, syringes, ampoules and cartridges. See also Figure 1.Note 1 to entry: These containers are made from borosilicate or soda-lime-silica glass.3.5filling volumedefined volume of water to fill the test specimenNote 1 to entry: For the determination of the filling volume, see 7.2. The filli
32、ng 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.3.6borosilicate glasssilicate glass having a very high hydrolytic resistance due to its composition containing significant amounts of boric ox
33、ideNote 1 to entry: 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 to entry: Neutral glass is a borosilicate glass having a very high hydrolytic resistance and a high thermal shock
34、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 HCF1 of this part of ISO 4802.3.7soda-lime-silica glasssilicate glass containing a mass fraction up to approximately 15 %
35、 of alkali metal oxides, mainly sodium oxide, and a mass fraction up to about 15 % of alkaline earth oxides, mainly calcium oxideNote 1 to entry: Containers made from this glass will have a moderate hydrolytic resistance due to the chemical composition of the glass, and comply with hydrolytic resist
36、ance container class HCF3.7DIN ISO 4802-2:2017-02 a) Example of a glass cylinder for pen-injectors (see ISO 13926-1)b) Example of an injection vial made of glass tubing (see ISO 8362-1)c) Example of a glass barrel (see ISO 11040-4)d) Example of a stem cut ampoule with constriction (see ISO 9187-1)Fi
37、gure 1 Examples of containers8DIN ISO 4802-2:2017-02 3.8surface treatmenttreatment 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: Surf
38、ace treatment is used, for example, in order to change a soda-lime-silica glass container of hydrolytic resistance class HCF3 to a container of hydrolytic resistance class HCF2 container. Treated containers are rinsed before use.3.9vialsmall, flat-bottomed container, made from tubing or from moulded
39、 glassNote 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 PrincipleThis method of test is a surface test applied to glass containers as produced and/or as delivere
40、d.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 ReagentsDuring the test, unless oth
41、erwise stated, use only reagents of recognised 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 boros
42、ilicate 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
43、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 S/cm, determined at 25 C by an in-line conductivity meter.NOTE 2 This description is based on the European Pharmacop
44、oeia 3.2.112. In the European Pharmacopoeia, water prepared as described above is designated water R1.NOTE 3 Water of Grade 2 according to ISO 36962is suitable for this test.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
45、, 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!9DIN ISO 4802-2:2017-02 5.5 Purified water prepared by distillation, by ion exchange, by reverse osmosis or by any other suitable method from water having dri
46、nking water quality.NOTE 1 See national or regional regulation on water intended for human consumption.NOTE 2 Water that corresponds to Grade 3 according to ISO 3696 is suitable.NOTE 3 In the European Pharmacopoeia 3.2.112, water as described above is designated water R.5.6 Spectrochemical buffer so
47、lution (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 ch
48、loride, 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 m
49、g/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 g/ml of sodiu
