Dr Will's apparatus has been modified by Dr Robertson,[A] of the Royal Gunpowder Factory, Waltham Abbey. The form of the apparatus used by him is shown in Fig. 51.
~CO_{2} Holders.~—Although objection has been taken to the use of compressed CO_{2} in steel cylinders on account of the alleged large and variable amount of air present, it has, nevertheless, been found possible to obtain this gas with as little as 0.02 per cent. of air. Frequent estimations of the air present in the CO_{2} of a cylinder show that even with the commercial article, after the bulk of the CO_{2} has been removed, the residual gas contains only a very small amount of air, which decreases in a gradual and perfectly regular manner. For example, one cylinder which gave 0.03 per cent. of air by volume, after three months' constant use gave 0.02 per cent. The advantage of using CO_{2} from this source is obvious when compared with the difficulty of evolving a stream of gas of constant composition from a Kipps or Finkener apparatus. A micrometer screw, in addition to the main valve of the CO_{2} cylinder, is useful for governing the rate of flow. A blank experiment should be made to ascertain the amount of air in the CO_{2} and the correction made in the readings afterwards.
[Footnote A: Jour. Soc. Chem. Ind., June 30, 1902, p. 819.]
[Illustration: Fig 51.—Will's Apparatus for Testing Nitro-cellulose]
~Measurement of Pressure and Rate of Flow.~—Great attention is paid to the measurement of the rate of flow of gas, which is arrived at by counting with a stop-watch the number of bubbles of gas per minute in a small sulphuric acid wash bottle. A mercury manometer is introduced here, and is useful for detecting a leak in the apparatus. The rate of flow that gives the most satisfactory results is 1,000 c.c. per hour. If too rapid it does not become sufficiently preheated in the glass spiral, and if too slow there is a more rapid decomposition of the nitro-cellulose by the oxides of nitrogen which are not removed.
~Decomposition Tube.~—This is of the form and dimensions given by Dr Will (15 mm. wide and 10 cm. high), the preheating worm being of the thinnest hydrometer stem tubing. The ground-in exit tube is kept in position by a small screw clamp with trunnion bearings.
~Bath.~—To permit of two experiments being carried on simultaneously, the bath is adapted for two decomposition tubes, and is on the principle of Lothar Meyer's air bath, that is, the bath proper filled with a high- flashing hydrocarbon oil, and fitted with a lid perforated with two circular holes for the spiral tubes, is surrounded by an asbestos-covered envelope, in the interior of which circulate the products of combustion of numerous small gas jets. The stirrer, agitated by a water motor, or, better still, a hot-air engine, has a series of helical blades curved to give a thorough mixing to the oil. Great uniformity and constancy of temperature are thus obtained. The bath is fitted also with a temperature regulator and thermometer.
~Reduction Tube~—This is of copper, and consists of two parts, the outer tube and an inner reaching to nearly the bottom of the former. Into the inner tube fits a spiral of reduced copper gauze, and into the annular space between the tubes is fitted a tightly packed reduced copper spiral. At the bottom the inlet tube dips into a layer of copper oxide asbestos, on the top of which is a layer of reduced copper asbestos. Through the indiarubber cork passes a glass tube, which leads the CO_{2} and nitrogen out of the reduction tube. As the portion of the tube containing the spirals is heated to redness, water jackets are provided on both inner and outer tubes to protect the indiarubber cork.
~Nitrogen Measuring Apparatus.~—The measuring tube with zigzag arrangement is used, having been found very economical in potash. It is most convenient to take readings by counterbalancing the column of potash solution and reading off the volume of gas at atmospheric pressure. For this purpose the tap immediately in front of the measuring tube is momentarily closed, this having been proved to be without ill effect on the progress of the test. In all experiments done by this test the air correction is subtracted from each reading, and the remainder brought to milligrams of nitrogen with the usual corrections. As objection has frequently been taken to the test on the ground of difficulty in interpreting the results obtained, Dr Robertson made a series of experiments for the purpose of standardising the test, and at the same time of arriving at the condition under which it could be applied in the most sensitive and efficient manner. A variety of nitro-celluloses having been tested, there were chosen as typical, of stable and unstable products, service gun-cotton on the one hand, and an experimental gun- cotton, Z, on the other. The first point brought out by these experiments was the striking uniformity of service gun-cotton, first in regard to the rectilinear nature of the curve of evolution of nitrogen, and secondly in regard to the small range within which a large number of results is included, 15 samples lying between 6.6 and 8.7 mgms. of nitrogen evolved in four hours. In the case of service gun-cotton, little difference in the rate of evolution of nitrogen evolved is obtained on altering the rate of passage of CO_{2} gas through the wide range of 500 c.c. per hour to 2,500 c.c. per hour. With Z gun-cotton (see Fig. 52), however, the case is very different. Operating at a rate of 1,000 c.c. of CO_{2} per hour, a curve of nitrogen evolution is obtained, which is bent and forms a good representation of the inherent instability of the material as proved to exist from other considerations. Operating at the rate of 1,500 c.c. per hour, as recommended by Dr Will, the evolution of nitrogen is represented by a straight line, steeper, however, than that of service gun-cotton. The rate of passage of CO_{2} was therefore chosen at 1,000 c.c. per hour, or two-thirds of the rate of Dr Will, and this rate, besides possessing the advantage claimed of rendering diagnostic the manner of nitrogen evolution in Z gun-cotton, has in other cases been useful in bringing out relationships, which the higher rate would have entirely masked.
[Illustration: Fig. 52.—Dr. Robertson's results.]