The one-tube preamplifier, or cathode follower described by Jordan and Bell (5) was found satisfactory, although frequent replacement of electron tube 6AK5 seemed necessary. A f'entralab ceramic condenser with a 5000-volt rating was used for decoupling.Amplifier. The Atomic Instrument Co.'s Model 204A is considered excellent in this application. From the various outputs it was possible, simultaneously, to count pulses, to view them on an oscillograph, and to monitor them with a counting rate meter. A discriminator, which is essential in neutron counting, is a part of this amplifier. It was used to determine the optimum gain or pulse discrimination level for obtaining reproducible results.Scaler. A conventional Higinbotham scaler was used, with a scale of 64 or 512 according to the counting rate. A DuMont Type 248A oscillograph with triggered sweep of various durations was exceedingly helpful throughout the work.
Nitroglycerin determination in methyl isobutyl ketone results in low values. Most of the solvent is removed by evaporation and the titration is conducted in dimethylformamide as described. In Table II, MNT was titrated in dimethylformamide, and nitrocellulose and nitroglycerin were titrated in ethylenediamine. The results in Table III, were obtained by dissolving the TXT in methyl isobutyl ketone and the inorganic nitrate in acetic acid. Aliquots were taken from the volumetric solutions and titrated (the TNT at 10 ml. per minute and the inorganic nitrate at 20 ml. per minute).The synthetic mixtures were made up on a percentage basis using c.p. grade ingredients with the exception of nitroglycerin (18.40% nitrogen) and nitrocellulose (12.52% nitrogen) which were assayed by means of the nitrometer.
The object of this investigation was to find a simple and convenient volumetric method for the determination of cobalt in complex compounds. The sample is prepared by ignition to the oxide and fusion with pyrosulfate. The solution is treated with potassium bicarbonate and hydrogen peroxide to form a carbonato complex of cobalt(III) which IN CONNECTION with the synthesis of various cobalt(III) complexes, a simple and rapid method for the determination of cobalt in these compounds was desired. Lack of interferences was of secondary importance because of the freedom from other metals.One of the simplest of the existing procedures was first investigated by Job ( 6), who oxidized the cobalt with hydrogen peroxide in the presence of potassium bicarbonate to give a soluble green carbonato complex. This he reduced with ferrous pyrophosphate, the excess of which was titrated with potassium permanganate solution.Metzi (7) also formed this soluble green complex as a step in iiis procedure. However, as a subsequent step he decomposed the complex by boiling in sodium hydroxide solution to give cobalt
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