Cold bath assembly

Figure 3 Refrigerated Immersion Probe Cold Bath Assembly.

The yellow slurry is stirred for 2-3 hours at — 15°. With rapid nitrogen flushing, the addition funnel is replaced with an adapter attached to a nitrogen line, the thermometer and mechanical stirrer are replaced with stoppers, and all joints are secured with standard-taper-joint clips (A. H. Thomas Co.). The apparatus shown in Fig. 1 is assembled and filled with nitrogen. The joints B and C are secured with standard-taper-joint clips. With nitrogen flushing through stopcock 1 and the reaction flask, the Dry Ice condenser is removed from the reaction flask and replaced by joint A the joint is secured with a joint clip. Care must be taken to support the reaction flask suitably, and it must be replaced in the cold bath. The filter is im-... 

After this has been achieved the sample is flame sealed at position 1. All the glass parts and the high vacuum seal are removed under continuous cooling from the high-pressure capillary, and the filling capillary is resealed at position 2. The capillary glass sample cell is then screwed into the copper-beryllium autoclave, which is precooled, while the assembly remains in the cold bath until the assembly is complete. 

Place 29 g. of n-caproamide (Section 111,109) into a 200 ml. distilling flask, and assemble the apparatus shown in Fig. Ill, 28, 1. Remove the trap momentarily and introduce 45 g. (27-5 ml.) of redistilled thionyl chloride no apparent reaction takes place in the cold. Warm the mixture on a water bath or by means of a small flame for 1 hour. Arrange the apparatus for distillation and distil oflF the excess of thionyl chloride (t.c., until the temperature reaches about 90°) and allow to cool. When cold, transfer the residue to a 100 ml. distilling flask (1). Distil from an air bath (Fig. II, 5, 3) the n-capronitrile passes over at 161-163° (2). The yield is 21 g. 

Oydobutanone. A 2-1. three-necked flask is fitted with an efficient mechanical stirrer and a water-cooled condenser assembled for downward distillation to which is attached a 250-rnl. receiver with a side arm. Two cold traps are attached consecutively to the distillation apparatus as shown in Figure 2 (Not 12). The receiver is immersed in an ice-water bath, and the traps are immersed in dry ice-acetone. To the flask is... 

HN03 to the bomb, place the crucible in the electrode support of the bomb, and attach the fuse wire. Assemble the bomb and add oxygen to a pressure of 24 atm (gage). Place the bomb in the calorimeter (a cold water bath in a large stainless steel beaker is also satisfactory) and ignite the sample using appropriate safety precautions ordinarily employed in bomb calorimetry work. 

Into a freshly charged cell, as previously prepared, place 300 milliliters (10.1 fluid oz.) of ice-cold tap water into the anode compartment (clay pot), and then add and dissolve 50 grams (1.8 oz.) of sodium chlorate into this water. Thereafter, place 500 milliliters (17 fluid oz.) of ice-cold tap water into the cathode compartment, and then add and dissolve 50 grams (1.8 oz.) of sodium chlorate there into. Thereafter assemble the cell as illustrated below, and then place the cell into an ice bath, and then begin the electrolysis process. The desired dimensions of the titanium electrodes may vary, but it is recommended to use rectangular bars of 10 to 15 millimeters in width of surface area (0.39 inches by 0.59 inches), and the electrodes should be placed about 127 millimeters apart (5 inches). The current should be 1.5 to 2.7 volts DC current at about 50 amps. Over voltage should be minimum, and the cell temperature should be kept below 5 Celsius at all times. Electrolyze the solution for about 18 to 24 hours. 

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