ASTM D1839 Standard Test Method for Amyl Nitrate in Diesel Fuels
6. Apparatus
6.1 Absorption Cells, matched, having a 1.000 more or less 0.002-cm light path.
6.2 Distillate Collector, borosilicate glass with standard taper joints and sealed-in funnel (Fig. 1).
6.3 Electric Heating Mantle, to fit a 300-mL round-bottom flask, and having a variable transformer.
6.4 Lunge-type Pipet, 2-mL capacity.
NOTE 2 - A 2.5-mL hypodermic syringe, with scabbard, can be used instead of the Lunge pipet.
6.5 Reflux Condenser (Allihn-type), borosilicate glass, 300 mm long, with standard-taper joints.
6.6 Round-Bottom Flask, of borosilicate glass and having a 300-mL capacity.
6.7 Separatory Funnel, Squibb-type, 125-mL capacity.
6.8 Shaking Machine, automatic, capable of 250 oscillations/min.
6.9 Spectrophotometer, capable of measuring absorption in the region of 452 nm.
7. Reagents
7.1 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 Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. 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.
7.2 Purity of Water - Unless otherwise specified, references to water shall be understood to mean reagent water as defined as Type II or III in Specification D1193.
7.3 Acetone (Warning - Extremely flammable. Vapors can cause flash fire. Harmful if inhaled.).
7.4 Amyl Nitrate - Any mixture of nitrate esters of primary amyl alcohol.
7.5 Diethyl Ether (Warning - Extremely flammable. Vapors can cause flash fire. Harmful if inhaled.).
7.6 Sodium Hydroxide Solution (20 g/L) - Dissolve 20 g of sodium hydroxide (NaOH) pellets in water and dilute to 1 L.
7.7 Sulfuric Acid (5 + 3) - Slowly add, with stirring, 500 mL of nitrate-free concentrated sulfuric acid (H2SO4, rel dens 1.84) to 300 mL of water. The m-xylenol solution must be added before the H2SO4, otherwise low or negative results will be obtained. Cool before use.
7.8 m-Xylenol Solution - Dilute 4 mL of m-xylenol (2,4-dimethylphenol) to 100 mL with acetone. Prepare fresh each day.
8. Sampling
8.1 Samples shall be taken in accordance with the appropriate instructions in Practice D4057.
