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苯基萤光酮法测定微量锗,早有报道,当加入Triton X-100后,可达到增敏增溶之目的,但当室温低于10℃时,该体系仍会产生混浊,故本方法提出加入一定量的聚乙烯醇,从而保证在较低的室温条件下,仍可正常显色。本方法灵敏度虽然很高,但Sn(Ⅳ)、Sb~(3+)、Ti(Ⅳ)、Nb(Ⅴ)、Mo(Ⅵ)等高价金属离子干扰锗的测定。在研究过程中发现柠檬酸、甘露醇、抗坏血酸和EDTA等不干扰测定,并可分别掩蔽上述干扰离子,而当以过氧化钠熔融试样时,Sb~(3+)被氧化成Sb(Ⅴ)消除了干扰。试验证明,加入10ml EDTA(0.01M),20μg锗的回收率可达99％以上。在选择的条件下,0—20μg/50ml范围内符合比尔定律,双
Phenylfluorone method for the determination of trace germanium has long been reported. When Triton X-100 is added, the sensitization and solubilization can be achieved. However, when the room temperature is lower than 10 ° C, the system still produces turbidity. Therefore, the present method Proposed to join a certain amount of polyvinyl alcohol, thus ensuring that at lower room temperature, the color can still be normal. Although the sensitivity of this method is high, the determination of germanium by high valent metal ions such as Sn (Ⅳ), Sb 3+, Ti (Ⅳ), Nb (Ⅴ), Mo (Ⅵ) During the course of the study, it was found that citric acid, mannitol, ascorbic acid and EDTA did not interfere with the determination and were able to mask the above interfering ions, respectively. When the sample was melted with sodium peroxide, Sb 3+ was oxidized to Sb Elimination of interference. Test proved that, adding 10ml EDTA (0.01M), 20μg germanium recovery rate of up to 99%. Under the chosen conditions, Beer’s law, double, is obeyed in the range 0-20 μg / 50ml