Chemistry Research Laboratory, Department of Chemistry, Shri Shivaji Mahavidyalaya, Barshi 413401, Maharashtra, India.
Chemistry Research Laboratory, Department of Chemistry, Shri Shivaji Mahavidyalaya, Barshi 413401, Maharashtra, India.
Spectrochim Acta A Mol Biomol Spectrosc. 2020 Dec 15;243:118814. doi: 10.1016/j.saa.2020.118814. Epub 2020 Aug 11.
An easy and selective method has been developed for the extractive spectrophotometric determination of ruthenium(III) with 4-(4'-flurobenzylideneimino)-3-methyl-5-mercapto-1,2,4-triazole (FBIMMT) as a chelating reagent. The basis of the method is the formation of stable complex of 'soft base' FBIMMT with 'soft acid' ruthenium(III). The reagent FBIMMT in n-butanol easily forms extractable yellow coloured complex with ruthenium(III) in acetate buffer of pH 4.8. The absorbance of [Ru(III)-FBIMMT] complex is measured at 394 nm against the reagent blank. Good linearity range of concentration up to 27.0 μg mL of ruthenium(III) is attained with correlation coefficient R = 0.998. The optimum concentration range is 6 to 27.0 μg mL which is deduced by Ringbom's plot. The apparent molar absorptivity found to be 2.75 × 10 L mol cm. Some additional characteristics such as limit of detection (LOD = 0.48 μg mL), limit of quantification (LOQ = 1.19 μg mL), and Sandell's sensitivity (SS = of 0.0367 μg cm) are also estimated. The composition of [Ru(III)-FBIMMT] complex has been established from Job's continuous variation method, mole ratio method, and log-log plot method. The specificity towards ruthenium(III) is well studied and appropriate masking agents are applied wherever required to boost it. The intra-day and inter-day precision values are found to be brilliant with % relative standard deviation of 0.52 and 0.68 respectively with % accuracy within the range of 99.00-100. The method is effectively used for determination of ruthenium(III) from water samples, binary and ternary synthetic mixtures, fissium alloy samples and catalyst materials. A scheme for sequential group separation of ruthenium(III), palladium(II) and osmium(VIII) has also been developed. The reproducible results of the present method confirm that the method has a good potential for quantitative determination of ruthenium(III) from various matrices.
一种简单而选择性的方法已经被开发出来，用于用 4-(4'-氟苯亚甲基亚氨基)-3-甲基-5-巯基-1,2,4-三唑 (FBIMMT) 作为螯合试剂，从医学专业学术文献中提取和分光光度法测定三价钌。该方法的基础是“软碱”FBIMMT 与“软酸”三价钌形成稳定的配合物。试剂 FBIMMT 在正丁醇中很容易在 pH 值为 4.8 的醋酸盐缓冲液中与三价钌形成可萃取的黄色配合物。[Ru(III)-FBIMMT] 配合物的吸光度在 394nm 处测定，以试剂空白为参比。在 27.0μg·mL 的钌(III)浓度范围内，达到了良好的线性关系，相关系数 R=0.998。最佳浓度范围是 6 到 27.0μg·mL，这是由 Ringbom 图推断出来的。表观摩尔吸光系数为 2.75×10 L·mol·cm。还估计了一些其他特性，如检测限 (LOD=0.48μg·mL)、定量限 (LOQ=1.19μg·mL) 和 Sandell 的灵敏度 (SS=0.0367μg·cm)。通过 Job 连续变化法、摩尔比法和对数-对数图法确定了[Ru(III)-FBIMMT] 配合物的组成。对三价钌具有良好的选择性，并在需要时应用适当的掩蔽剂来增强其选择性。日内和日间精密度值非常出色，相对标准偏差分别为 0.52%和 0.68%，准确度在 99.00-100.0%范围内。该方法有效地用于水样、二元和三元合成混合物、锇合金样品和催化剂材料中三价钌的测定。还开发了一种顺序分组分离三价钌、钯(II)和锇(VIII)的方案。本方法重现性好，证实该方法具有从各种基质中定量测定三价钌的良好潜力。
