電子管制御式硫黄及びハロゲン分析装置

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The mechanism of automatically controlled combustion(1, 2, 3) was applied on the microdetermination of halogens and sulfur. The sample was burnt in a stream of oxygen in the presence of platinum contact, and the amount of halogens or sulfur was determined from the weight increase of two silver-net-rolls (each 5cm long), on which halogens or sulfur were caught as AgHal or Ag2SO4, respectively. The analytical condition recommended were as follows: 1) Silver-net-rolls were recommended to be reduced electrolytically after the analysis. 2) Silver rolls must be cooled on a chrome plated copper cooler (Fig. 4). 3) The sample could be burnt at the same rate as in the case of the C-H determination in a stream of oxygen of 10cc/min. But 200cc of oxygen must be passed for the expelling and 4_??_6 mg of sample was necessary for the determination of halogens. 4) For the determination of halogens (Cl, Br, I), silver roll must be heated at 400_??_450°. 5) The same temperature could be applied for the determination of sulfur when a silver roll of 10cm (or two 5cm long rolls) was used. But if the length of the roll was 5cm, the temperature must be at about 550° and the rate of the oxygen flow must be reduced to 5cc/min. 6) Separated analysis of halogens and sulfur was possible, but was very troublesome. 7) Platinum contacts must be reactivated after about 50 analyses with a hot solution of 20% HNO2. 8) When the rear part of the quarz reaction tube was stained yellow by the silver (halide ?), the tube must be cut off and a new one be welded.
社団法人日本農芸化学会の論文

電子管制御式硫黄及びハロゲン分析装置

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