ASTM D565-99(R2019) pdf free download

ASTM D565-99(R2019) pdf free download.Standard Test Method for Carbonizable Substances in White Mineral Oil
1. Scope
1.1 This test method covers white mineral oil (Mineral Oil USP and Light Mineral Oil NF) to determine whether it conforms to the standard ofquality required for pharmaceutical use as defined by the United States Pharmacopeia and the National Formulary, or the Food and Drug Administration. 1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.2.1 Exception—Dimension requirements for the color comparator in Fig. 1 are in SI and inch-pound units. 1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appro- priate safety, health, and environmental practices and deter- mine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 6. 1.4 This international standard was developed in accor- dance with internationally recognized principles on standard- ization established in the Decision on Principles for the Development of International Standards, Guides and Recom- mendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
5. Apparatus
5.1 Test Tube, as shown in Fig. 1, of heat-resistant glass fitted with a well-ground glass stopper, the stopper and the tube bearing identical and indestructible numbers. The tube shall be 140 mm 6 2 mm in length and between 14.5 mm and 15.0 mm in outside diameter, and shall be calibrated at the 5 mL 6 0.2 mL and 10 mL 6 0.2 mL liquid levels. The capacity of the tube with stopper inserted shall be between 13.6 mL and 15.6 mL. A rolled edge can be provided for suspending the tube on the cover of the water bath. 5.2 Water Bath, suitable for immersing the test tube above the 10 mLline equipped to maintain a temperature of100 °C 6 0.5 °C. The bath shall be provided with a cover of any suitable material with holes approximately 16 mm in diameter through which the test tubes can be suspended. 5.3 Color Comparator, of a suitable type for observing the color of the acid layer in comparison with the reference standard color solution. The size and shape of the comparator are optional, but the size and shape of the apertures shall conform to the dimensions prescribed in Fig. 1.
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Commit- tee on Analytical Reagents of the American Chemical Society, where such specifications are available. 5 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity ofWater—Unless otherwise indicated, references to water shall be understood to mean distilled water or water of equal purity conforming to Type III of Specification D1193. 6.3 Cobaltous Chloride Solution (0.25 M)—Prepare a solu- tion of hydrochloric acid (HCl) (Warning—Causes burns. Vapor extremely irritating.) by mixing 30 mL of concentrated HCl with 1170 mL of water. Slowly add the acid to the water. Dissolve 65 g 6 1 g of cobaltous chloride hexahydrate (CoCl 2 ·6H 2 O) in the HCl solution to make 1000 mL of solution. Using a pipet, transfer 5 mL of this solution to a 250 mL iodine flask. Prepare a solution of sodium hydroxide (NaOH) (Warning—Corrosive. Can cause severe burns or blindness. Evolution of heat produces a violent reaction or eruption upon too rapid a mixture with water.) by mixing 5 g of NaOH with 20 mL of water. Add 15 mL of this NaOH solution to the iodine flask. Add 5 mL of hydrogen peroxide (H 2 O 2 ) (3 % v/v). Boil for 10 min 6 1 min, cool, and add 2 g of potassium iodide (KI). Prepare a solution of H 2 SO 4 (Warning—Causes burns. Vapor extremely irritating. Strong oxidizer.) by mixing 6 mL of H 2 SO 4 with 18 mL of water. Slowly add the acid to the water (see Note 1). Add 20 mL of this H 2 SO 4 solution to the flask.) When the precipitate has dissolved, titrate the liberated iodine with 0.100 M sodium thiosulfate (Na 2 S 2 O 3 ) solution, using starch solution as an indicator.