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1、IS0 4802-2 INTERNATIONAL STANDARD INTERNATIONAL ORGANIZATION FOR STANDARDIZATION ORGANISATION INTERNATIONALE DE NORMALISATION MEX,fJYHAPO,QHAR OPrAHM3AMR fl0 CTAHAPTM3AklM Glassware - Hydrolytic resistance of the interior surfaces of glass containers - Part 2 : Determination by flame spectrometry an
2、d classification Verrerie - Rksistance hydrolytique des surfaces internes des rkcipients en verre - Pat-tie 2 : D b) a classification of glass containers according to the hydrolytic resistance of the interior surfaces determined by the methods specified in this part of IS0 4802. NOTE - The hydrolyti
3、c resistance container class HC obtained by the flame spectrometry is comparable with the class HC obtained accor- ding to IS0 4802-1, although the individual test values are not equal. 2 Applicability This part of IS0 4802 applies to containers, such as bottles, vials, ampoules, flasks, beakers, et
4、c., made for instance from soda-lime-silica glass, whether surface-treated or not, or from borosilicate glass or neutral glass. This part of IS0 4802 does not apply to double-ended ampoules or to the classification of closed ampoules. 3 Normative references The following standards contain provisions
5、 which, through reference in this text, constitute provisions of this part of IS0 4802. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this part of IS0 4802 are encouraged to investigate the possibility of appl
6、ying the most recent editions of the standards shown below. Members of IEC and IS0 main- tain registers of currently valid International Standards. IS0 385-l : 1984, Laboratory glassware - Burettes - Part 7 : General requirements. IS0 385-2 : 1984, Laboratory glassware - Burettes - Part 2 : Burettes
7、 for which no waiting time is specified. IS0 719 : 1985, Glass - Hydrolytic resistance of glass grains at 98 T - Method of test and classification. IS0 720 : 1985, Glass - Hydrolytic resistance of glass grains at 121 OC - Method of test and classification. IS0 1042 : 1983, Laboratory glassware - One
8、-mark volumetric flasks. IS0 3898 : 1987, Water for analytical laboratory use - Specification and test methods. IS0 3819 : 1985, Laboratory glassware - Beakers. 4 Definitions For the purposes of this part of IS0 4802, the following defini- tions shall apply. 4.1 container : Any article made from bor
9、osilicate, neutral or soda-lime-silica glass, such as bottles, vials, ampoules and articles especially 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 therma
10、l shock resistance and 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. 1 -,-,- IS0 4602-2 : 1966 (El 4.3 neutral glass : A silicate glass containing significant a
11、mounts of boric oxide, usually between 5 % and 13 % (m/m), aluminium and/or alkaline earth oxides, and 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. 4.4
12、soda-lime-silica glass : A silicate glass containing up to approximately 15 % (m/m) of alkali metal oxides - mainly sodium oxide - and up to about 15 % (m/m 1 of alkaline earth oxides, mainly calcium oxide. Containers made from this glass will have a moderate hydrolytic resistance due to the chemica
13、l composition of the glass, and comply with hydrolytic resistance container class HC 3 or hydrolytic 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
14、to the treatment, and comply with hydrolytic 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
15、 alkali earth metal ions). 4.6 brimful capacity : 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). 4.7 filling volume : The volume of water to be filled into the test specimen. For vials, bottles and l
16、ipped 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). 4.8 vial; phial : Small, flat-bottomed container, made from tubing or from moulded glass; normally thick-
17、walled and with a capacity up to about 50 ml. NOTE - Vials are normally sealed with a closure made from a material other than glass, and not by flame-sealing. 4.9 bottle : Flat-bottomed container, made from moulded glass; normally thick-walled and with a capacity usually of more than 50 ml. Bottles
18、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. 4.16 ampoule : Normally flat-bottomed container, made from thin-walled tubing, and having stems in many different forms. Ampoules ar
19、e intended to be closed after filling by flame- sealing. Capacity normally up to 25 ml. Types : open and closed ampoules (see figure I). 5 Principle The methods of test are surface tests normally applied to glass containers as delivered. Filling of the containers to be tested with specified water to
20、 a specified capacity and heating of the containers loosely capped under specified conditions. Measurement of the degree of the hydrolytic attack by flame spectrometric analysis of the extrac- tion solutions. 6 Reagents During the test, unless otherwise stated, use only reagents of recognized analyt
21、ical grade. 6.1 Test water, consisting of grade 1 water or grade 2 water, which complies with the requirements specified in IS0 3696. 6.2 Hydrochloric acid, solution, c(HCI) = 2 mol/l. 6.3 Hydrochloric acid, solution, c(HCI) = 6 mol/l (= 1 + I). 6.4 Hydrofluoric acid, c(HF) = 22 mol/l (i.e. = 400 g
22、HF/I solution). 6.5 Distilled water or water of equivalent purity (grade 3 water complying with the requirements specified in IS0 3696). 6.6 Spectrochemical buffer solution (caesium chloride solution, CsCI). Dissolve 80 g of caesium chloride in approximately 300 ml of test water (6.11, add 10 ml of
23、hydrochloric acid (6.3) and transfer to a 1 000 ml volumetric flask (7.3). Dilute to the mark with the test water (6.1) and mix. 6.7 Stock solutions 6.7.1 Dry sodium chloride, potassium chloride and calcium carbonate at 110 OC f 5 OC for 2 h. Prepare aqueous stock solutions, using the test water (6.
24、1), directly from the chlorides and from the calcium carbonate, after dissolving in just suffi- cient excess of hydrochloric acid so that all solutions have con- centrations of 1 mg/ml, calculated as sodium oxide, potassium oxide and calcium oxide, respectively. 6.7.2 Commercially available standard
25、 solutions may also be used. 2 IS0 4802-2 : 1999 (El a) -b . . b) d) Figure 1 - Examples of typical open a) and b)l and closed c) and d)l ampoules 6.8 Standard solutions 6.8.1 Prepare standard solutions by diluting the stock solu- tions (6.7) with the test water (6.1) to obtain concentrations suitab
26、le for establishing the reference solutions in an ap- propriate manner, e.g. with concentrations of 20 pg/ml of sodium oxide, potassium oxide and calcium oxide, respectively. 6.8.2 Commercially available standard solutions may also be used. 6.9 Reference solutions The reference solutions for establi
27、shing the calibration graph (set of calibration solutions) shall be prepared by diluting suitable concentrated standard solutions (6.8) with the test water (6.1). They should cover normally the optimum working ranges of the specific elements according to the instrument used for the measurement. Typi
28、cal concentration ranges of the reference solutions are - for determination by flame atomic emission spectro- scopy (FAES) of sodium oxide and potassium oxide : up to 10 pg/ml - for determination by flame atomic absorption spectro- metry (FAAS) of sodium oxide and potassium oxide : up to 3 pg/ml - f
29、or determination by flame atomic absorption spectro- metry (FAAS) of calcium oxide : up to 7 pg/ml For the measurement on containers of hydrolytic resistance container classes HC 1, HC 2 or HC B (borosilicate or highly resistant glasses), the reference solutions shall be used without addition of the
30、 spectrochemical buffer solution (6.6). For the measurement of containers of hydrolytic resistance container classes HC 3 or HC D (soda-lime-silica glasses), the reference solutions shall contain 5 % (V/v) of the spectro- chemical buffer solution (6.6). 3 IS0 4802-2 : 1988 (El 7 Apparatus Ordinary l
31、aboratory 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 specified in 9.2. It should preferably be equipped with a constant-pressure regulator or other means of maintain- ing the temperature at 12
32、1 “C 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, a pressure gauge, a pressure-release safety device, a vent- cock, and a rack for supporting the samples. The autoclave vessel and ancill
33、ary equipment shall be thoroughly cleaned before use. 7.2 Burettes, having a suitable capacity according to the analytical procedure to be used and complying with the re- quirements specified for class A burettes in IS0 385-2 and made of glass of hydrolytic resistance grain class HGA 1 as specified
34、in IS0 7201). 7.3 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 IS0 1042. 7.4 Water bath, capable of being heated to approximately 80 = C. 7.5 Flame atomic absorption (FAA9 or flame atomic emission (F
35、AES) 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 ox- ide/acetylene gas supply and burner for measuring calci
36、um. FAES instruments shall be equipped with air/propane or air/acetylene gas supplies and burners for measuring sodium and potassium. 7.5 Beakers, having a suitable capacity and complying with the requirements specified in IS0 3819. Before use, each new beaker shall be pretreated by subjecting it to
37、 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, transparent material of any convenient shape, but with a central hole ap- proximately 5 mm in diameter. The strike-plate shall be large enough to f
38、it snugly on and completely cover the sealing sur- face of the container the brimful capacity of which is to be measured. * 2,5 x 10s N/mz = 0,25 MPa = 2,5 bar 8 Sample preparation 8.1 Sample size For each container capacity to be tested, the number of con- tainers which are to be measured separatel
39、y is specified in table 1. Table 1 - Number of containers for the determination of the hydrolytic resistance by flame spectrometry methods Capacity volume corresponding to filling volume (see 8.2)1 8.2 Determination of the filling volume 8.2.1 Flat-bottomed containers up to 30 ml capacity (except am
40、poulesl Select six containers at random from the sample lot and remove any dirt or packaging debris by shaking the container. Place each dry container on a flat, horizontal surface and allow to reach a temperature of 22 OC + 2 OC. Cover each container with a strike-plate (7.7) with the hole position
41、ed approximately central to the mouth of the container. Fill each container with distilled water (6.5) at 22 OC 2 2 Y from a burette (7.21, through the hole in the strike-plate, until the meniscus is just level with the bottom of the hole. Ensure that no air bubbles are trapped at the water/strike-p
42、late interface. Then read the volume of water filled in from the burette to two decimal places. This volume is the brimful capacity of the container. Calculate the mean value of the results from the six containers. Then calculate 90 % of this mean brimful capacity to one decimal place. This volume i
43、s the filling volume for the par- ticular sample lot. 8.2.2 Flat-bottomed containers of 30 ml capacity and greater 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 p
44、ackaging debris by shaking the containers. Allow the dry con- tainers to reach a temperature of 22 OC f 2 OC. Cover each container with a suitable strike-plate (7.7) and weigh each of the empty covered containers to the nearest 0,l g. Remove the strike-plate and fill the container nearly to the top
45、with distilled water (6.5) 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 for the particular sample lot. 8.2.3 Round-bottomed containers (except ampoules) Select six containers (
46、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 containers. Allow the dry con- tainers to reach a temperature of 22 OC f 2 OC. Fix each con- tainer vertica
47、lly 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 filling volume for the par- ticular sample lot. 8.2.4 Lipped containers Wrap adhesive plastics tape arou
48、nd the rim of the containers such that the tape around the lip is level with the rim. Weigh the container with its strike-plate (7.7) in place, then fill and reweigh as described in 8.2.2, without taking the strike-plate Off. 8.2.5 Ampoules Place at least six dry ampoules at 22 OC f 2 OC on a flat,
49、horizontal surface and fill them with the distilled water (6.5), at the same temperature, from a burette (7.21, until the water reaches point A, where the body of the ampoule declines to the shoulder (see figure 2). Read the capacities to two decimal places and calculate the mean value. This volume, expressed to one decimal place, is the filling volume and shall be filled in ampoules of the same lot. 9 Procedure This procedure shall be completed within one working day. 9.1 Cleaning of samples This cleaning process shall be completed from the
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