ガラス製リングオブン法による銅基,スズ基合金少量試料中の銅,鉄の定量
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概要
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The Weisz Ring Oven<SUP>1)</SUP> and apparatus by Ballczo<SUP>2)</SUP> have been known to be effective for qualitative and quantitative analysis of microsubstance, but they have many faults. The authers have presented an apparatus made of hard glass which can be handled more easily, noncorrosive, keeps, warm better and is more stable than the previous apparatus. Some experiments were carried out by using the present a glass ring oven and the results were compared with those obtained by using the Weisz Ring Oven.<BR>Bathocuproine and bathophenanthroline were used as detection reagents of copper and iron. The effect of the coexisting ions is smaller by the use of these reagents than by the reagents used in the conventional methods<SUP>4)6)</SUP> and thus a more specific and selective detection and determination is possible by the present method (Limit of detection, Cu : 0.005 μg, Fe : 0.009 μg, Range of determination, Cu : 0.013.0 μg, Fe : 0.024.0 μg). The sample solution is spotted on a filter paper (55 mmφ). After copper, lead and cadmium ions are fixed by exposing the disk to H<SUB>2</SUB>S gas stream and silver is fixed by exposing it to HCl vapor. Then it is placed on a oven and heated at 90°C, and iron is allowed to diffuse out of the disk into a ring zone by dropping 0.010.05<I>N</I> HCl solution. For copper, no H<SUB>2</SUB>S gas exposure was made, it was diffused out of disk into a ring zone by dropping 0.010.05 <I>N</I> HCl. The latent rings of iron and copper are sprayed by a 1 : 1 solution of bathocuproine and hydroquinon, and 1 : 1 solution of bathophenanthroline and hydroquinon, respectively. And exposed to ammonium vapor to develop color. Standard rings prepared from samples containing various amount of each metal. The contents of copper and iron in copper base and tin base alloys were measured. The limit of the error was ±1% when the results obtained by the present method were compared with those by polarography. The whole procedures took about 10 minutes. The present method may be applied for the analysis of samples in other field.
- 社団法人 日本分析化学会の論文
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