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1、INTERNATIONAL STANDARD INTERNATIONAL ORGANIZATION FOR STANDARDIZATION ORGANISATION INTERNATIONALE DE NORMALISATION MEXflYHAPOaHAR OPrAHM3AMR n0 CTAHflAPTMBAl4M Glassware - Hydrolytic resistance of the interior surfaces of glass containers - Part 1 : Determination by titration method and classificati
2、on Verrerie - R b) a classification of glass containers according to the hydrolytic resistance of the interior surfaces determined by the method specified in this part of IS0 4902. NOTE - The hydrolytic resistance container class HC obtained by titration is comparable with the class HC obtained acco
3、rding to IS0 4802-2, although the individual test values are not equal. 2 Applicability This part of IS0 4902 applies to containers, such as bottles, vials, ampoules, flasks, beakers, etc., made for instance from soda-lime-silica glass, whether surface-treated or not, or from borosilicate glass or n
4、eutral glass. This part of IS0 4902 does not apply to double-ended ampoules. 3 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this part of IS0 4902. At the time of publication, the editions indicated were valid. All sta
5、ndards are subject to revision, and parties to agreements based on this part of IS0 4902 are encouraged to investigate the possibility of applying the most recent editions of the standards listed below. Members of IEC and IS0 main- tain registers of currently valid International Standards. IS0 395-l
6、 : 1964, Laboratory glassware - Burettes - Part 1 : General requirements. IS0 366-2 : 1964, Laboratory glassware - Burettes - Part2 : Burettes for which no waiting time is specified. IS0 646 : 1977, Laboratory glassware - One-mark pipettes. IS0 719 : 1966, Glass - Hydrolytic resistance of glass grai
7、ns at 98 T - Method of test and classification. IS0 720 : 1966, Glass - Hydrolytic resistance of glass grains at 121 T - Method of test and classification. IS0 1773 : 1976, Laboratory glassware - Boiling flasks (narrow-necked). IS0 3696 : 1997, Water for analytical laboratory use - SpecKcation and t
8、est methods. IS0 3619 : 1966, Laboratory glassware - Beakers. 4 Definitions For the purposes of this part of IS0 4902, the following defini- tions shall apply. 4.1 container : Any article made from borosilicate, neutral or soda-lime-silica glass, such as bottles, vials, ampoules and articles especia
9、lly intended for laboratory or pharmaceutical use, which is capable of being filled. 4.2 borosilicate glass : A silicate glass containing between 5 and 13 % (m/m) of boric oxide, having a high thermal shock resistance and a very high hydrolytic resistance due to its com- position. Containers properl
10、y made from this glass comply with hydrolytic resistance container class HC 1 of this International Standard. 1 -,-,- IS0 4802-I : 1988 (El 4.3 neutral glass : A silicate glass containing significant amounts of boric oxide, usually between 5 and 13 % (mlm), aluminium and/or alkaline earth oxides, an
11、d having a very high hydrolytic resistance due to its composition. Containers properly made from this glass comply with hydrolytic resistance container class HC 1 of this International Standard. 5 Principle This method of test is a surface test normally applied to glass containers as delivered. Fill
12、ing of the containers to be tested with specified water to a specified capacity and heating of the containers loosely capped under specified conditions. Measurement of the degree of the hydrolytic attack by titration of the extraction solutions. 4.4 soda-lime-silica glass : A silicate glass containi
13、ng up to approximately 15 % (m/m) of alkali metal oxides - mainly sodium oxide - and up to about 15 % (m/m) of alkaline earth oxides, mainly calcium oxide. 6 Reagents Containers made from this glass will have a moderate hydrolytic resistance due to the chemical composition of the glass, and comply w
14、ith hydrolytic resistance container class HC 3 or hvdrolvtic resistance container class HC D. After sur- face treatment (see 4.51, soda-lime-silica glass containers of hydrolytic resistance container class HC 3 will have a very high hydrolytic resistance, due to the treatment, and comply with hydrol
15、ytic resistance container class HC 2. 4.5 surface treatment : Treatment of the internal surface of soda-lime-silica 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). 4.6 brimful c
16、apacity : The volume of water required to fill a container, placed on a flat, horizontal surface, until the meniscus just touches the strike-plate (see 7.7). During the test, unless otherwise stated, use only reagents of recognized analytical grade. 6.1 Test water, consisting of grade 2 water, which
17、 complies with the requirements specified in IS0 3696 and which has been freed from dissolved gases, such as carbon dioxide, by boiling for at least 15 min in a boiling flask of fused silica or borosilicate glass. The boiling flask shall be pretreated once as specified in 9.2 before it is used for t
18、he first time. When tested immediately before use, this test water shall be neutral to methyl red, i.e. it shall produce an orange-red (not a violet-red or yellow) colour corresponding to pH 5,5 f 0,l when four drops of the methyl red indicator solution (6.5) are added to 50 ml of the test water. 4.
19、7 filling volume : The volume of water to be filled into the test specimen. For vials, bottles, and lipped containers, it is defined as 90 % of the brimful capacity. For ampoules, it is defined as the volume up to the height where the body of the ampoule declines to the shoulder (see figure 2). NOTE
20、 - The water, so coloured, may also be used as the reference solution (see 9.3). Such test water can normally be stored for 24 h in a stoppered flask without change of the pH value. 4.8 vial; phial : Small, flat-bottomed container, made from tubing or from moulded glass; normally thick-walled and wi
21、th a capacity up to about 50 ml. ATTENTION - Grade 1 water, complying with the re- quirements specified in IS0 3696, will not comply with the above specified pH requirement and shall therefore not be used for the determination by titration. NOTE - Vials are normally sealed with a closure made from a
22、 material other than glass, and not by flame-sealing. 6.2 Hydrochloric acid, standard volumetric solution, c(HCI) = 0,Ol mol/l. 4.9 bottle : Flat-bottomed container, made from moulded glass; normally thick-walled and with a capacity usually of more than 50 ml. 6.3 Hydrochloric acid, solution, c(HCI)
23、 = 2 mol/l. Bottles may be of circular or other geometric cross-section. NOTE - Bottles are normally sealed with a closure made from a material other than glass, and not by flame-sealing. 6.4 Hydrofluoric acid, c(HF) = 22 mol/l (i.e. = 400 g HF/I solution). 4.10 ampoule : Normally flat-bottomed cont
24、ainer, made from thin-walled tubing, and having stems in many different forms. Ampoules are intended to be closed after filling by flame sealing. Capacity normally up to 25 ml. Types : open and closed ampoules (see figure I). 6.5 Methyl red, indicator solution. Dissolve 25 mg of the sodium salt of m
25、ethyl red (C15H14N3Na02) in 100 ml of the test water (6.1). 6.6 Distilled water or water of equivalent purity (grade 3 water complying with the requirements specified in IS0 3696). 2 IS0 4802-l : 1999 (E) a) Figure 1 - Examples of typical open a) and bll and closed cl and d)l ampoules 7 Apparatus 7.
26、3 Conical flasks, having a capacity of 100 ml and 250 ml and complying with the requirements of IS0 1773. c / . b) /- t h - dl Ordinary laboratory apparatus, and 7.1 Autoclave or steam sterilizer, capable of withstanding a pressure of at least 2,5 x 105 N/mz* and of carrying out the heating cycle sp
27、ecified in 9.2. It should preferably be equipped with a constant-pressure regulator or other means of maintain- ing the temperature at 121 OC f 1 OC. The vessel shall have an internal diameter of at least 300 mm and shall be equipped with a heating device, a thermometer or a calibrated thermocouple,
28、 a pressure gauge, a pressure-release safety device, a vent- cock, and a rack for supporting the samples. The autoclave vessel and ancillary equipment shall be thoroughly cleaned before use. 7.2 Burettes, having a suitable capacity of 50 ml, 25 ml, 10 ml or 2 ml, complying with the requirements spec
29、ified for class A burettes in IS0 385-2 and made of glass of hydrolytic resistance grain class HGA 1 as specified in IS0 72011, The capacity of the burettes shall be chosen according to the expected consumption of hydrochloric acid (6.2). * 2,5 x 105 N/m2 = 0,25 MPa = 2.5 bar Before use, each new fl
30、ask shall be pretreated by subjecting it to the autoclaving conditions described in 9.2. 7.4 Pipettes, having a suitable capacity and complying with the requirements specified for class A pipettes in IS0 648. 7.5 Water bath, capable of being heated to approximately 80 T. 7.6 Beakers, having a suitab
31、le capacity and complying with the requirements specified in IS0 3819. Before use, each new beaker shall be pretreated by subjecting it to the autoclaving conditions described in 9.2. 7.7 Strike-plates (for measuring the brimful capacity of small bottles and bottles), made of rigid, inert, transpare
32、nt material of any convenient shape, but with a central hole ap- proximately 5 mm in diameter. The strike-plate shall be large enough to fit snugly on and completely cover the sealing sur- face of the container the brimful capacity of which is to be measured. 1) Glass of hydrolytic resistance grain
33、class IS0 719-HGB 1 adequately meets the requirements of class HGA 1 specified in IS0 720. 3 IS0 4802-I : 1988 (E) 8 Sample preparation 8.1 Sample size The number of containers to be tested depends on the capacity of the container, the volume of extraction solution necessary for one titration and th
34、e number of titration results required. It shall be calculated according to the requirements given in table 1. Table 1 - Number of containers for the determination of the hydrolytic resistance by titration Capacity volume Minimum Volume of corresponding to number of extraction filling volume contain
35、ers solution Number of (see 8.2)1 for one for one titrations titration titration ml ml Up to and including 3 10 25,0 1 From 3 up to and including 30 5 %O 2 From 30 up to and including 100 3 100.0 2 From 100 upwards 1 100,o 3 8.2 Determination of the filling volume 8.2.1 Flat-bottomed containers up t
36、o 30 ml capacity (except ampoules) Select six containers at random from the sample lot and remove any dirt or packaging debris by shaking the containers. Place each dry container on a flat, horizontal surface and allow to reach a temperature of 22 OC f 2 OC. Cover each container with a strike-plate
37、(7.7) with the hole positioned approximately central to the mouth of the container. Fill each container with distilled water (6.6) at 22 OC this value is the mean brimful capacity of the containers. Calculate 90 % of this mean brimful capacity to one decimal place. This volume is the filling volume
38、for the particular sample lot. 8.2.3 Round-bottomed containers (except ampoules) Select six containers (having a capacity less than or equal to 100 ml) or three containers (having a capacity greater than 100 ml) at random from the sample lot and remove any dirt or packaging debris by shaking the con
39、tainers. Allow the dry con- tainers to reach a temperature of 22 OC F 2 OC. Fix each con- tainer vertically in an appropriate device and determine the brimful capacity according to 8.2.1 or 8.2.2, respectively. Then calculate 90 % of the mean brimful capacity to one decimal place. This volume is the
40、 filling volume for the par- ticular sample lot. 8.2.4 Lipped containers Wrap adhesive plastics tape around the rim of the containers such that the tape around the lip is level with the rim. Weigh the container with the strike-plate (7.7) in place, then fill and reweigh as described in 8.2.2, withou
41、t taking the strike-plate Off. 8.2.5 Ampoules Place at least six dry ampoules at 22 YI account shall be taken of the size and wall thickness of the samples and the type of glass from which the samples are made in order to avoid losses by thermal shock. The cooling time shall not exceed 30 min. Start
42、 with the determinations after cooling. WARNING - Take care that the cooling tap water does not contact the loose foil caps. This is very dangerous, especially in vials. Combine the extraction solutions of the containers (see column 2 of table I). When emptying small stemmed ampoules there is a dang
43、er of neutralization of the solution by absorption of carbon dioxide (COz), from the atmosphere. To obviate this, invert the ampoules and heat the bases gently with a cool flame. In the case of the combined extraction solutions from containers having a capacity less than or equal to 3 ml, pipette a
44、volume of 25,0 ml (see column 3 of table I) into a conical flask (7.3) having a capacity of 100 ml. In the case of the combined extraction solutions from containers having a capacity from 3 to 30 ml or from 30 to 100 ml (see column 1 of table I), pipette volumes of 50,O and 100,O ml, respectively (s
45、ee column 3 of table I), into separate conical flasks (7.3) having a capacity of 250 ml. In the case of samples with a capacity above 100 ml (see column 1 of table 11, pipette a volume of 100,O ml from each container into separate conical flasks (7.3) having a capacity of 250 ml. Prepare reference s
46、olutions by pipetting volumes, equivalent to those taken from the extraction solutions, of the test water IS. 1) into conical flasks (7.3) having a capacity commensurate with the size of the containers being tested. Add two drops of methyl red indicator solution (6.5) to each 25 ml of test water (6.
47、1). Add two drops of methyl red indicator solution (6.5) to each flask for each 25 ml of extraction solution and titrate with hydrochloric acid (6.2) until the colour matches exactly that of coloured reference solutions. Titration values of less than 1,O ml shall be expressed to two decimal places,
48、titration vaiues greater than or equal to 1,0 ml to one decimal place. 5 -,-,- IS0 4602-l : 1966 (El 9.4 Testing to determine whether the containers Apply the surface etching treatment as specified in 9.4.1, and have been surface-treated test the samples as specified in 9.2, and 9.3. 9.4.1 Vials and
49、 bottles NOTE - The hydrolytic resistance of the interior surface of vials and bottles made from soda-lime-silica glass can be considerably increased by treating those surfaces during the course of production. If it is necessary to determine whether or not a container has been surface-treated, the samples previously tested shall be used. Fill the samples with the mixture of 1 volume of hydrofluoric acid (6.4) and 9 volumes of hydrochloric acid (6.3) to the brim- ful point. Allow the filled samples to stand a