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在现行的国内外钢铁化学分析标准方法中,测定锑的分光光度法为亮绿法和甲基紫及孔雀绿分光光度法。上述方法中,为消除干扰离子,提高方法的精确度,均需用苯或甲苯萃取,以硫酸锰为载体富集后显色,故颇感不便。本文着重研究了以苯基萤光酮为显色剂,在非离子表面活性剂TritonX—100和聚乙烯醇的存在下,直接测定锑的最佳条件,于0.24～0.72N的硫酸介质中,为防止锑的水解,加入酒石酸,使之成为酒石酸盐,从而保证在较低酸度条件,加入3ml苯基萤光酮(0.1％),5mlTritonx—100(5％)和3ml聚乙烯醇(0.5％)能形成多元络合物,3分钟即可显色完全,络合物可持续稳定1小时,0～30Pg/50ml范围内符合比耳定律,根据工作曲线计算得摩尔吸光系数2510nm=7.5×10~4。Fe、Zr、Mo、Ti,Nb、W等高价金属离子干扰测定,但上述离子除W外,可分别加入抗坏血酸、柠檬酸、硫酸羟胺和甘霹醇等消除干扰。应用于钢铁(不含钨)中微量锑的直接测定,获得较满意的结果。
In the current standard methods for chemical analysis of steel at home and abroad, the determination of antimony spectrophotometry bright green and methyl violet and malachite green spectrophotometry. In the above method, in order to eliminate interfering ions and improve the accuracy of the method, it is necessary to use benzene or toluene to extract, and to enrich and collect the color with the manganese sulfate as a carrier, it is inconvenient. This paper focuses on the determination of the optimum conditions for the direct determination of antimony with phenylfluorone as color reagent in the presence of nonionic surfactant TritonX-100 and polyvinyl alcohol. In 0.24 ~ 0.72N sulfuric acid medium, To prevent the hydrolysis of antimony, tartaric acid is added to make it a tartrate, thereby ensuring the addition of 3 ml of phenylfluorone (0.1%), 5 ml of Triton X-100 (5%) and 3 ml of polyvinyl alcohol (0.5% ) Can form multi-complex, 3 minutes to complete color development, the complex can be sustained and stable for 1 hour, 0 ~ 30Pg / 50ml Beer’s law consistent with the law, calculated according to the working curve molar absorption coefficient of 2510nm = 7.5 × 10 ~ 4. Fe, Zr, Mo, Ti, Nb, W and other high-value metal ions interfere with the determination, but the above ions in addition to W, were added ascorbic acid, citric acid, hydroxylamine sulfate and glycerol, etc. to eliminate interference. Used in steel (non-tungsten) in the direct determination of trace antimony, get more satisfactory results.