@article{oai:kanazawa-u.repo.nii.ac.jp:00031263, author = {松本, 健 and 西尾, 学 and 三崎, ゆかり and 寺田, 喜久雄}, issue = {328}, journal = {分析化学 = Japan analyst}, month = {Mar}, note = {酸化スズ(IV),酸化アンチモン(III)及び酸化ビスマス(III)の分解法として,ヨウ化アンモニウム融解法の適用を検討し迅速簡便な方法を確立した.すなわちパイレックスガラス製試験管に酸化物試料とヨウ化アンモニウム約2gを入れ,触媒として白金の小片を加えて混合し,冷却管を取り付けた後,バーナーの小さな炎で加熱する.約1分間の加熱で分解は十分であり,スズ(IV),アンチモン(III)及びビスマス(III)はそれぞれのヨウ化物として試料マトリックスから昇華分離し,冷却管中に完全に捕集される.昇華物を2M塩酸で溶解し,溶液中のスズ,アンチモン及びビスマスの量を黒鉛炉原子吸光法で定量する.本法を環境生物試料,鉱石及びたい積物試料中の微量のスズ,アンチモン及びビスマスの定量に応用した.定量値は他の研究者の報告値とよく一致した. A finely ground sample (SnO_2 Sb_2O_3, Bi_2O_3, soils, ores, sediments and ashes of biological materials) was accurately weighed and placed in a simple decompo sition tube (Pyrex glass, 15mm o.d., 45mm length) together with an excess amount of ammonium iodide and a small piece of platinum wire as a catalyst. The tube was attached to the cold trap (Pyrex glass, 20 mm o. d., 330 mm length) with the aid of hooks made on the wall of both tubes. While rotating, the bottom of the decomposition tube was gently heated with a small flame of the fish-tail burner for about one minute. The sublimates containing tin, antimony and bismuth iodides were condensed on the lower part of the inside wall of the cold trap. When the evolution of iodine ceased, the tube was removed from the flame and allowed to cool. The cold trap was detached from the decomposition tube and sublimates on the tube were completely dissolved in 20 ml of 2 M hydrochloric acid. The solution was collected into a 25 ml volumetric flask and made to the volume with 2 M hydrochloric acid. If further dilution is necessary, use of 2 M hydrochloric acid is preferable. Finally, the concentrations of tin, antimony and bismuth were determined by graphite furnace atomic absorption spectrometry at the 224.6 nm, 306.7 nm and 217.6nm lines, respectively. The three metals did not interfere with each other in the atomic absorption measurement of each metal. Low contents of tin, antimony and bismuth in biological, environmental and geological materials were determined by the pro posed method and the results obtained were in goodagreement with those reported by other authors. The proposed method is simple, fast and accurate for the decomposition of the sparingly soluble SnO_2, Sb_2O_3, and Bi_2O_3 and the determination of these elements., 金沢大学イノベーション創成センター}, pages = {141--145}, title = {ヨウ化アンモニウム融解による酸化スズ(IV),酸化アンチモン(III)及び酸化ビスマス(III)の分解と分析への応用}, volume = {31}, year = {1982} }