ASTM D3712 Standard Test Method of Analysis of Oil-Soluble Petroleum Sulfonates by Liquid Chromatography
6. Apparatus
6.1 Chromatographic column, made of glass and consisting of a reservoir and separator section, and fitted with a TFE-fluorocarbon stopcock with a 2-mm bore, as shown in Fig. 1. A column with a detachable reservoir connected by a standard-taper joint can be used.
6.2 Steam Bath.
6.3 Vacuum Desiccator, shielded.
6.4 Vacuum Oven, capable of being maintained at 100°C (212°F) and connected to 559 to 635 mm (22 to 29 in.) Hg vacuum.
6.5 Muffle Furnace, capable of operating at 800 to 1000°C (1500 to 1800°F).
6.6 Dish, platinum, 100-mL capacity.
6.7 Distillation Apparatus, as described in Test Method D95.
6.8 Water Bath, capable of being maintained at 25 +/- 0.2°C (77 +/- 0.3°F).
6.9 Pycnometer, as shown in Fig. 2. To calibrate, weigh to the nearest 1 mg with cap in place; then fill with distilled water at 15 to 20°C (60 to 68°F) and place in water bath at 25 +/- 0.2°C (77 +/- 0.3°F). After 30 min, adjust the water meniscus at the top of the neck so it is exactly level. To obtain a flat meniscus, add a minute amount of wetting agent to the water surface. Remove the pycnometer from the bath, and dry the outside. Replace the cap and weigh to the nearest 1 mg. Record the mass of water contained as Wc.
7. Reagents and Materials
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 Chloroform (Warning - Flammable, Health Hazard.).
7.3 Ethyl Alcohol (95 %) - Either pure grain or denatured ethyl alcohol conforming to Formula 3A of the U.S. Bureau of Internal Revenue (Warning - Flammable. Denatured alcohol cannot be made nontoxic.).
7.4 Ethyl Ether (Warning - Extremely flammable. Harmful if inhaled. May cause eye injury. Effects may be delayed. May form explosive peroxides. Vapors may cause flash fire. Moderately toxic. Irritating to skin.).
7.5 Filter Paper, slow-filtering, ashless, gravimetric.
7.6 Hydrochloric Acid (Concentrated) - (Warning - Poison. Corrosive. May be fatal if swallowed. Liquid and vapor cause severe burns. Harmful if inhaled.).
7.6.1 Hydrochloric Acid, Dilute (1 + 1) - (See Warning in 7.6.) One volume of concentrated hydrochloric acid (HCl) is added to 1 volume of water.
7.6.2 Hydrochloric Acid, Dilute (1 + 3) - (See Warning in 7.6.) One volume of concentrated hydrochloric acid (HCl) is added to 3 volumes of water.
7.7 Isopropyl Alcohol (99 Mass %) - Water content shall be 0.9 mass % maximum. (Warning - Flammable.)
7.7.1 Isopropyl Alcohol, Dilute (1 + 1) - One volume of 99 mass % isopropyl alcohol is diluted with 1 volume of water.
7.8 Methyl Orange Indicator Solution - Dissolve 1.0 g of methyl orange in water and dilute to 1 L.
7.9 Phenolphthalein Indicator Solution - Dissolve 1 g of phenolphthalein in 100 mL of 50 mass % ethyl alcohol.
7.10 Silica Gel, 250 to 74 µm (60 to 200-mesh).
7.11 Sodium Hydroxide Solution, Standard (0.1 mol/L) (Warning - Corrosive. Can cause severe burns or blindness. Evolution of heat produces a violent reaction or eruption upon too rapid mixture with water.) - Prepare and standardize a 0.1 mol/L aqueous, carbonate-free, NaOH solution.
7.12 Sodium Sulfate, Anhydrous, Crystalline.
7.13 Sodium Sulfate Solution - Dissolve 240 g of sodium sulfate (Na2SO4) in water and dilute to 1 L.
7.14 Sulfuric Acid (relative density 1.84) - Concentrated sulfuric acid (H2SO4), 36 mol/L. (Warning - Poison. Corrosive. Strong oxidizer. Contact with organic material may cause fire. May be fatal if swallowed. Liquid and vapor cause severe burns. Harmful if inhaled. Contact with water liberates large amounts of heat. Spillage may cause fire.
7.14.1 Sulfuric Acid Solution, Standard (0.1 mol/L) - Prepare and standardize a 0.1 mol/L aqueous sulfuric acid (H2SO4).
