By W. T. Elwell
E-book via Elwell, W T wooden, D F
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Extra resources for Analysis of the New Metals. Titanium, Zirconium, Hafnium, Niobium, Tantalum, Tungsten and Their Alloys
L-type, three-limb (7 mm) T2 to T6. Straight-bore (7 mm) All joints and taps must be free from leaks. " Apiezon" W wax for joints including the rubber sleeve (4), and "Apiezon" N grease for taps are recommended. 2. 4), and place a flask of liquid nitrogen over the cold finger (11). Close taps T2, T3, T4 and T5, and diffuse a small volume of hydrogen into the apparatus through the osmosis-tube (10), heated to about 300°C (Note 1). , the difference in level between mercury at the 01-ml calibration mark and in the 1-mm bore limb.
Tin forms a yellow-coloured compound with the reagent, and this complex has a considerable absorption at 420 m/i. Interference by tin, up to at least 2 0 % , is overcome by using an alternative acid mixture to dissolve the sample, followed by the removal of tin as volatile stannic bromide. Copper above about 0-025 % causes low and erratic results, but it is precipitated during solution of titanium, and its effect is eliminated [ 3 0 ]   36 ANALYSIS OF THE NEW METALS if the sample solution is filtered before oxidation with nitric acid.
When the pressure is constant, as shown by the Pirani gauge (after about 2 min), remove the small furnace and measure the residual pressure (p) as before, on the McLeod gauge. The difference (P4 — p) between the pressure of the evolved gas and the residual pressure is due to hydrogen. Use the value (P4 — p) in place of P4 in the calculation. 7. Shutting Down the Apparatus Close all taps and the needle valve. Switch off the furnaces, diffusion pumps and Pirani gauge. Switch off the rotary-pump and simultaneously open tap T6.