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P-C-111C <br /> 4.5.6.2 Ethylene glycol diethyl ether. <br /> 4.5.6.2. 1 Preparation of sample. In a liter separatory funnel , acidify <br /> 500 ml . of the compound with concentrated hydrochloric acid. Cool during <br /> addition of the acid. Add a large excess of potassium carbonate and let <br /> separate. Transfer the top layer to a glass stoppered Erlenmeyer flask. <br /> Add anhydrous potassium carbonate in small portions, shaking thoroughly, <br /> until some solid salt remains. Transfer the liquid to another flask and <br /> similarly add more anhydrous potassium carbonate, until free flowing granu- <br /> lar potassium carbonate remains in excess . Let settle for one hour or more, <br /> rechecking the excess carbonate for free flowing character. If necessary, <br /> add more carbonate. <br /> 4.5.6.2.2 Test method. Use the dried material from 4.5.6.2. 1 and test in <br /> accordance with ASTM D 56 except heat from room temperature to 125°F. in 10 <br /> to 12 minutes. Apply test flame for the first time at 125°F. A flash at <br /> this time shall be considered evidence of ethylene glycol diethyl ether or <br /> compounds of similar or higher vapor pressure. <br /> 4.5.7 Condition in container. <br /> 4.5.7.1 Type 1. The compound as received shall be thoroughly mixed by <br /> hand, stirring for 5 minutes with a rod or spatula reaching to the bottom <br /> of the original container. Examine the contents for undispersed solids and <br /> note whether any material adheres to the bottom or sides of the container <br /> or has caked or failed to redisperse. Promptly transfer 1 liter of the <br /> mixed compound to a container and observe whether gelation or thickness of <br /> the compound makes pouring difficult. Add 1 liter of distilled water and <br /> stir gently for 15 minutes. Note ease with which precipitate is dispersed. <br /> Determine quantity of insoluble matter as in 4.5.7.3. <br /> 4.5.7.2 Type 11. The compound as received shall be thoroughly mixed. <br /> Transfer to a 2 liter bottle, noting ease of pouring. Determine quantity <br /> of insoluble matter as in 4.5.7.3. <br /> 4.5.7.3 Insoluble matter. Filter 100.0 ml. of the thoroughly mixed com- <br /> pound, Type—1 diluted or Type 11 as received, through a medium porosity <br /> fritted glass crucible. Prepare the crucible with a glass fiber filter disc <br /> ,pr with an asbestos mat, wash with distilled water, then ethanol, and dry <br /> for 30 minutes at 110°C. Weigh to 0.1 mg. When all the compound has been <br /> filtered, wash container and crucible with about 30 ml. distilled water, <br /> transferring insoluble matter to the crucible. Wash crucible with 50 ml. <br /> ethanol, using small portions in both cases. Dry crucible at 110°C. , cool <br /> in a desiccator and weigh. The increase in weight shall be reported as <br /> grams insoluble matter per 100 ml. compound. <br /> 14 <br />