The following tests are designed to determine the resistance to water attack of new (not previously used) glass containers. The degree of attack is determined by the amount of alkali released from the glass under the influence of the attacking medium under the conditions specified. This quantity of alkali is extremely small in the case of the more resistant glasses, thus calling for particular attention to all details of the tests and the use of apparatus of high quality and precision. The tests should be conducted in an area relatively free from fumes and excessive dust.

Type	General Description1	Type of Test	Limits
			Size,2 mL	mL of 0.020 N Acid
I	Highly resistant, borosilicate glass	Powdered Glass	All	1.0
II	Treated soda-lime glass	Water Attack	100 or less	0.7
			Over 100	0.2
III	Soda-lime glass	Powdered Glass	All	8.5
NP	General-purpose soda-lime glass	Powdered Glass	All	15.0
1  The description applies to containers of this type of glass usually available. 2  Size indicates the overflow capacity of the container.

Autoclave— For these tests, use an autoclave capable of maintaining a temperature of 121 ± 2.0, equipped with a thermometer, a pressure gauge, a vent cock, and a rack adequate to accommodate at least 12 test containers above the water level.

Mortar and Pestle— Use a hardened-steel mortar and pestle, made according to the specifications in the accompanying illustration.

Other Equipment— Also required are 20.3-cm (8-inch) sieves made of stainless steel including the Nos. 20, 40, and 50 sieves along with the pan and cover (see Sizes of Standard Sieve Series in Range of Interest under Particle Size Distribution Estimation by Analytical Sieving 786), 250-mL conical flasks made of resistant glass aged as specified, a 900-g (2-lb) hammer, a permanent magnet, a desiccator, and an adequate volumetric apparatus.

High-Purity Water— The water used in these tests has a conductivity at 25, as measured in an in-line cell just prior to dispensing, of not greater than 0.15 µS per cm (6.67 Megohm-cm). There must also be an assurance that this water is not contaminated by copper or its products (e.g., copper pipes, stills, or receivers). The water may be prepared by passing distilled water through a deionizer cartridge packed with a mixed bed of nuclear-grade resin, then through a cellulose ester membrane having openings not exceeding 0.45 µm.3 Do not use copper tubing. Flush the discharge lines before water is dispensed into test vessels. When the low conductivity specification can no longer be met, replace the deionizer cartridge.

Methyl Red Solution— Dissolve 24 mg of methyl red sodium in Purified Water to make 100 mL. If necessary, neutralize the solution with 0.02 N sodium hydroxide or acidify it with 0.02 N sulfuric acid so that the titration of 100 mL of High-Purity Water, containing 5 drops of indicator, does not require more than 0.020 mL of 0.020 N sodium hydroxide to effect the color change of the indicator, which should occur at a pH of 5.6.

Powdered Glass Test

Procedure— Transfer 10.00 g of the prepared specimen, accurately weighed, to a 250-mL conical flask that has been digested (aged) previously with High-Purity Water in a bath at 90 for at least 24 hours or at 121 for 1 hour. Add 50.0 mL of High-Purity Water to this flask and to one similarly prepared to provide a blank. Cap all flasks with borosilicate glass beakers that previously have been treated as described for the flasks and that are of such size that the bottoms of the beakers fit snugly down on the top rims of the containers. Place the containers in the autoclave, and close it securely, leaving the vent cock open. Heat until steam issues vigorously from the vent cock, and continue heating for 10 minutes. Close the vent cock, and adjust the temperature to 121, taking 19 to 23 minutes to reach the desired temperature. Hold the temperature at 121 ± 2.0 for 30 minutes, counting from the time this temperature is reached. Reduce the heat so that the autoclave cools and comes to atmospheric pressure in 38 to 46 minutes, being vented as necessary to prevent the formation of a vacuum. Cool the flask at once in running water, decant the water from the flask into a suitably cleansed vessel, and wash the residual powdered glass with four 15-mL portions of High-Purity Water, adding the decanted washings to the main portion. Add 5 drops of Methyl Red Solution, and titrate immediately with 0.020 N sulfuric acid. If the volume of titrating solution is expected to be less than 10 mL, use a microburet. Record the volume of 0.020 N sulfuric acid used to neutralize the extract from 10 g of the prepared specimen of glass, corrected for a blank. The volume does not exceed that indicated in Table 2 for the type of glass concerned.

Water Attack at 121

Procedure— Fill each container to 90% of its overflow capacity with High-Purity Water, and proceed as directed for Procedure under Powdered Glass Test, beginning with “Cap all flasks,” except that the time of autoclaving shall be 60 minutes instead of 30 minutes, and ending with “to prevent the formation of a vacuum.” Empty the contents from 1 or more containers into a 100-mL graduated cylinder, combining, in the case of smaller containers, the contents of several containers to obtain a volume of 100 mL. Place the pooled specimen in a 250-mL conical flask of resistant glass, add 5 drops of Methyl Red Solution, and titrate, while warm, with 0.020 N sulfuric acid. Complete the titration within 60 minutes after opening the autoclave. Record the volume of 0.020 N sulfuric acid used, corrected for a blank obtained by titrating 100 mL of High-Purity Water at the same temperature and with the same amount of indicator. The volume does not exceed that indicated in Table 2 for the type of glass concerned.

Arsenic

Arsenic 211— Use as the Test Preparation 35 mL of the water from one Type I glass container or, in the case of smaller containers, 35 mL of the combined contents of several Type I glass containers, prepared as directed for Procedure under Water Attack at 121: the limit is 0.1 µg per g.