Separatory funnel stopper

From this solution, prepare 25.0 mL of a 0.00025 M solution of iodine in water. Pour this entire solution into a 125-mL separatory funnel. Stopper the funnel. 

Stock solutions of 5% APCD (Fisher Scientific) are made daily in distilled deionized water and extracted at least three times with MIBK. Seawater samples are stored in acid-soaked, deionized, water-rinsed polypropylene bottles. All reagents used were reagent grade or the highest grade readily available. Polypropylene graduated cylinders and separatory funnel stoppers and Teflon stopcocks were used in all cases. 

To the separatory funnel add 5 mL of isatin solution and 10 mL of ferric sulfate-sulfuric acid solution. Stopper and shake for 2 min 15 s. Allow the phases to separate and draw off the lower H2SO4 layer into a 50-mL volumetric flask. Add 10 mL of H2SO4 to the separatory funnel, stopper, and shake for 30 5 s. Again draw off the lower H2SO4 layer into the 50-mL volumetric flask containing the first extract. Dilute to volume with H2SO4 and mix. 

About 150 ml. of concentrated sulphuric acid is placed in the larger funnel and 100 ml. of concentrated hydrochloric acid in the smaller separatory funnel. The latter is raised until the capillary tube is above the sulphuric acid, the capillary tube is filled with concentrated hydrochloric acid, and the stopper replaced. The rate of evolution of hydrogen chloride is controlled by regulation of the supply of hydro chloric acid this will continue until a volume of hydrochloric acid equal to that of the concentrated sulphuric acid has been used. The diluted sulphuric acid should then be removed and the apparatus recharged. The yield is 31-33 g. of hydrogen chloride per 100 ml. of concentrated hydro chloric acid. If more than an equal volume of hydrochloric acid is employed, the yield of gas decreases and continues to be formed for a tune after the stopcock has been closed. 

Separatory funnels. For many operations the globular form (compare Fig. II, 1, 5, c) with 14, 19 or 24 cone on the stem and 14 or 19 socket for the stopper, is convenient. For some purposes, e.g., when used on a three-necked flask or with a multiple adapter, the cylindrical... 

In a 250 ml. separatory funnel place 25 g. of anhydrous feri.-butyl alcohol (b.p. 82-83°, m.p. 25°) (1) and 85 ml. of concentrated hydrochloric acid (2) and shake the mixture from time to time during 20 minutes. After each shaking, loosen the stopper to relieve any internal pressure. Allow the mixture to stand for a few minutes until the layers have separated sharply draw off and discard the lower acid layer. Wash the halide with 20 ml. of 5 per cent, sodium bicarbonate solution and then with 20 ml. of water. Dry the preparation with 5 g. of anhydrous calcium chloride or anhydrous calcium, sulphate. Decant the dried liquid through a funnel supporting a fluted Alter paper or a small plug of cotton wool into a 100 ml. distilling flask, add 2-3 chips of porous porcelain, and distil. Collect the fraction boiling at 49-51°. The yield of feri.-butyl chloride is 28 g. 

Treat the distillate with 2 drops of glacial acetic acid (to destroy the phosphorus esters present) and redistil using the same apparatus as before except that the separatory funnel is replaced by a thermometer. Collect the liquid which passes over at 50-56°. Transfer the acetyl chloride to a weighed glass-stoppered bottle (since cork and rubber stoppers are attacked) and determine the weight. The yield is 22 g. 

Fit a 2-litre round-bottomed flask with a two-holed stopper carrying a separatory funnel and a reflux condenser (Fig. Ill, 71,1). Place 147 g. of finely-powdered sodium cyanide and 150 ml. of water in the flask and... 

Make a thin paste of 21 5 g. of finely-powdered o-tolidine (a commercial product) with 300 ml. of water in a 1-litre beaker, add 25 g. (21 ml.) of concentrated hydrochloric acid, and warm until dissolved. Cool the solution to 10° with ice, stir mechanically, and add a further 25 g. (21 ml.) of concentrated hydrochloric acid (1) partial separation of o tolidine dihydrochloride will occur. Add a solution of 15 g, of sodium nitrite in 30 ml. of water as rapidly as possible, but keep the temperature below 15° a slight excess of nitrous acid is not harmful in this preparation. Add the clear, orange tetrazonium solution to 175 ml. of 30 per cent, hypophosphorous acid (2), and allow the mixture to stand, loosely stoppered, at room temperature for 16-18 hours. Transfer to a separatory funnel, and remove the upper red oily layer. Extract the aqueous layer with 50 ml, of benzene. Dry the combined upper layer and benzene extract with anhydrous magnesium sulphate, and remove the benzene by distillation (compare Fig. II, 13, 4) from a Widmer or similar flask (Figs. II, 24, 3-5) heat in an oil bath to 150° to ensure the removal of the last traces of benzene. Distil the residue at ca. 3 mm. pressure and a temperature of 155°. Collect the 3 3 -dimethyldiphenyl as a pale yellow liquid at 114-115°/3 mm. raise the bath temperature to about 170° when the temperature of the thermometer in the flask commences to fall. The yield is 14 g. 

Dissolve 9-5 g. of hydrazobenzene (Section IV,87) in the minimum volume of ether (about 90 ml. are usually required), and add this solution in small portions from a separatory funnel to 100 ml. of ice-cold dilute hydrochloric acid (1 1) contained in a 350 ml. conical flask stopper the flask and shake after each addition. Benzidine hydrochloride separates out during the reaction. After all the hydrazobenzene has been introduced, add 50 ml. of concentrated hydrochloric acid and allow the mixture to stand for 30 minutes in ice water. Filter the benzidine hydrochloride at the pump, wash it first with 20 ml. of dilute hydrochloric acid (1 1) and then with two or three 20 ml. portions of ether (to dissolve any unchanged hydrazobenzene) (1). 

Equip a 500 ml. three-necked flask with a powerful mechanical stirrer and a separatory funnel leave the third neck open or loosely stoppered. Introduce, while the flask is cooled in a freezing mixture of ice and salt, 90 ml. of concentrated ammonia solution (sp. gr. 0 -88) and 54 g. (43 ml.) of pure (e.g., A.R.) carbon disulphide. Stir the mixture and run in 56 g. (55ml.)of pure aniline from the separatory funnel during about 20minutes stir for a further 30 minutes, and allow to stand for another 30 minutes. A heavy precipitate of ammonium phenyldithiocarbamate separates. Transfer the salt to a 5 litre round-bottomed flask by four extractions with 200 ml. portions of water. Add to the resulting solution, with... 

Dissolve 27 g. of potassium hydroxide in 25 ml. of water contained in a beaker or conical flask, and cool the solution to about 20° in ice water. Pour the solution into a 250 ml. reagent bottle, and add 30 g. (29 ml.) of pure benzaldehyde ("1) cork the bottle securely and shake the mixture vigorously until it has been converted into a thick emulsion. Allow the mixture to stand overnight or for 24 hours in the stoppered bottle. Add just sufficient water (about 105 ml.) to dissolve the potassium benzoate. Pour the liquid into a separatory funnel, rinse out the bottle with about 30 ml. of ether and add this ether to the solution in the funnel. Shake the... 

In figure 4 is shown how a separatory funnel and a pressure equalized addition funnel are made. The funnel part is just a PP funnel from the grocery store and what it is attached to is a stainless steel ball valve. See how the addition funnel is made by using a rubber stopper and an extra extension of tubing to the top of the funnel Well, that s how one can make a sealed addition funnel out of the ordinary glass separatory funnel that one gets with a distillation kit or from wherever. 

The apparatus illustrated in Fig. 3 is assembled, in a large hood if possible (Note 3). A is a 5- . round-bottom flask heated by a large ring burner and provided with a specially treated four-hole cork stopper covered with tin foil (Note 4). To these holes are fitted the column Z), the tube B reaching to the bottom of A, the specially bent tube C reaching up the inside of D, and the tube K connected with the tubes leading to the 2-I. separatory funnel H, so that the distance between the stopper of A and the stopcock of H is at least 100 cm. The bottom of the column D is of 20 mm. bore while the main portion is 30 mm. The side arm should be at least 85 cm. above the stopper of 4. The tube C... 

To the acid chloride, mechanically stirred and heated on the steam bath, is added 2.5 kg. (805 ml. 15.6 moles) of dry bromine as rapidly as it will react (Note 5). The addition requires about 12 hours. The contents of the flask are stirred and heated an additional 2 hours, transferred to a dropping funnel (Note 6), and added in a thin stream to 5 1. of absolute ethyl alcohol, which has previously been placed in a 12-1. flask provided with a stopper carrying an effleient reflux condenser, a separatory funnel, and a mechanical stirrer. The resulting vigorous reaction is controlled by external cooling. After the dibromoacid chloride has been added, the reaction mixture is allowed to stand at room temperature overnight and is then poured into 5 1. of cold water. The top alcoholic aqueous layer is decanted and extracted once with 8 1. of ether. The oily bottom layer is dissolved in the ether extract, washed first with 1 1. of a 2% sodium bisulfite solution, then with two 1-1. portions of 3% sodium carbonate solution, and finally with several portions of water. The ether solution is dried over 175 g. of potassium carbonate the solvent is distilled on the steam bath. The yield of residual ester (Note 7) amounts to 2260-2400 g. (91-97% of the theoretical amount). 

Frequently not all of the ammonia evaporates the first extraction should be by swirling in a separatory funnel without a stopper, and subsequent extractions should be done with frequent pressure release. 

In a one-liter separatory funnel, 94 g (0.215 mol) of scopolamine hydrobromide trihydrate was dissolved in 250 ml of water, made alkaline by shaking with 40 g (1 mol) of sodium hydroxide in 150 ml of water, and the free base immediately extracted with ether. As scopolamine is somewhat soluble in water, the aqueous layer was saturated with potassium carbonate and again extracted with ether. The combined ether extracts were dried over anhydrous magnesium sulfate and the ether removed by distillation, leaving 65 g (0.214 mol 100% yield) of nearly colorless oil. Then 100 g (1.05 mols) of cold methyl bromide was added to a chilled, 500-ml pressure flask containing the 65 g of scopolamine, the flask stoppered tightly with a clamp, and allowed to stand at room temperature for 96 hours. 

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