ASTM D3443-00(R2020) pdf free download

ASTM D3443-00(R2020) pdf free download.Standard Test Method for Chloride in Trichlorotrifluoroethane
1. Scope
1.1 This test method covers the determination of chloride in trichlorotrifluoroethane and other halocarbons that are liquid at room temperature. 1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.3 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 ofregulatory limitations prior to use. 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. Reagents
5.1 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. 2 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. 5.2 Purity ofWater—Unless otherwise indicated, references to water shall be understood to mean halide-free distilled water. 5.3 s-Diphenylcarbazone Solution—Dissolve 0.5 g of s-diphenylcarbazone, in 100 mL of methanol. 5.4 Silver Nitrate Solution—Dissolve 8.5 g of silver nitrate (AgNO 3 ) in 500 mL of water. 5.5 Standard Mercuric Acetate Solution—Dilute 40 mL of stock mercuric acetate solution, reagent 2, to 1000 mL and adjust the pH to 1.6 with nitric acid. Standardize as follows: 5.5.1 Pipet 10.00 mL of standard sodium chloride solution into a 250 mL Erlenmeyer flask. Add 20 mL of chloride-free water and 5 drops ofs-diphenylcarbazone solution. Titrate with standard mercuric acetate solution to the faint purple end point. Then:5.6 Standard Sodium Chloride Solution—Dissolve 0.0660 g of sodium chloride in water and dilute to 1000 mL. Pipet 25 mL of this solution into a 1000-mL volumetric flask, dilute to volume, and mix. One millilitre of this solution contains 1.00 µg of chloride ion.5.7 Stock Mercuric Acetate Solution—Dissolve 1.6 g of mercuric acetate in 500 mLofwater containing 3.5 mLofnitric acid. Dilute to 1000 mL and mix.
6. Procedure
6.1 Wash all glassware with chloride-free water until 10 mL ofthe washings show no trace of turbidity when 1 mL of silver nitrate solution is added. 6.2 Transfer 100 mL ofthe sample into a 250 mL separatory funnel, add 25 mL of chloride-free water to the sample and shake for 1 min. Transfer the sample to a second 250 mL separatory funnel and drain the water into a 125 mL Erlen- meyer flask. Repeat the extraction once with another 25 mL of water. Combine the water extracts in the Erlenmeyer flask. 6.3 Warm the water extract to 60 °C to drive off any remaining sample. Cool to room temperature. 6.4 Add 5 drops of s-diphenylcarbazone solution and titrate with standard mercuric acetate solution to the pale purple end point.
8. Precision and Bias
8.1 Repeatability (Single Analyst): The standard deviation of results (each the average of triplicates obtained by the same analyst on two different days) has been estimated to be 0.005 wt. ppm at four degrees offreedom. Two such values should be considered suspect (95 % confidence level) if they differ by more than 0.02 wt. ppm. 8.2 Reproducibility (Multilaboratory): The standard devia- tion of results (each the average of triplicates in four different laboratories) has been estimated to be 0.06 wt. ppm at three degrees of freedom. Two such values should be considered suspect (95 % confidence level) if they differ by more than 0.3 wt. ppm.