用指示纸用反射法和目测法测定复杂成分物体中的Pd(II)

Q4 Chemistry Analitika i Kontrol Pub Date : 2020-01-01 DOI:10.15826/analitika.2020.24.2.007
V. M. Ostrovskaya, E. A. Reshetnyak, O. Chernyshova, E. Bryleva
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引用次数: 0

摘要

提出了基于1-苯基-5-(3,4-二氢-6-甲基-4-氧- 3h -嘧啶-2-基)-甲酸-6-纤维素的rip - pd测试试剂指示纸,用于用吸附-反射法和目测法测定复杂组成物中钯的含量。介绍了RIP的合成工艺。给出了在pH 1.5 ~ 2.5条件下非均相指示剂反应形成的金属配合物的估计组成,保证了钯:试剂= 1:1的强制配位。当RIP与钯(II)离子相互作用时,黄色指示条变为不同强度的绿色。在所选择的条件下,对Pd(II)的检测和测定具有较高的选择性。借助“Ecotest-2040”便携式反射计,使用辐射波长为660 nm的红色LED进行反射测量。视觉测试采用色阶。在试纸条反应指示区(采用抽袋装置)上,提出了不加浓度和加浓度100倍、1000倍试验溶液三种模式进行指示剂反应。通过统计方法,估计了目测法测定Pd(II)的极限值(40、0.47、0.042 mg/l)。采用3s准则计算三种模式下的钯检出限分别为19、0.22、0.018 mg/l。所发现的极限浓度值与使用固相试剂的已知分析方法的计量特性相当。用原子发射法、分光光度法和重量法等独立的分析方法,证明了复杂组合物和药物中钯含量测定的正确性。便携式反射仪测定的Pd(II)浓度的相对标准偏差值不超过7%。
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Reflectometric and visual test determination of Pd(II) in objects of complex composition using the indicator paper
RIP-Pd-Test reagent indicator paper based on 1-phenyl-5-(3,4-dihydro-6-methyl-4-oxo-3H-pyrimidin-2-yl)-formazan-6-cellulose has been proposed for determining the palladium content using the sorption-reflectometry and visual-test methods in objects of complex composition. The RIP synthesis technique was described. The estimated composition of the metal complex formed as a result of the heterogeneous indicator reaction at pH 1.5–2.5 was indicated, and the forced coordination of palladium : reagent = 1:1 was ensured. When the RIP interacted with palladium (II) ions, the yellow indicator strip became green with different intensities. Under the selected conditions, the high selectivity for the detection and determination of Pd(II) was shown. With the help of the «Ecotest-2040» portable reflectometer, the reflectometry measurements were carried out using the red LED with the radiation wavelength of 660 nm. For the visual testing, the color scales were used. The indicator reaction was proposed to be carried out in three modes: without concentration and with concentration of the test solution in 100 and 1000 times on the reaction indicator zone of the paper strip (using the pocket pumping device). By the statistical method, the limit of Pd(II) determination for the visual test method (40, 0.47, 0.042 mg/l) was estimated. The palladium detection limit using the reflectometer (19, 0.22, 0.018 mg/l) for the three modes, respectively, was calculated by 3s criterion. The found values of the limiting concentrations were comparable with the metrological characteristics of the known analysis methods in which solid-phase reagents were used. The trueness of the palladium determinations in technological objects of complex composition and drugs has been proven by the independent methods - atomic emission, spectrophotometric and gravimetric methods of analysis. The value of the relative standard deviation of the determined Pd(II) concentration using the portable reflectometer did not exceed 7%.
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来源期刊
Analitika i Kontrol
Analitika i Kontrol Chemistry-Analytical Chemistry
CiteScore
0.90
自引率
0.00%
发文量
15
期刊介绍: Analitika i Kontrol is a scientific journal covering theoretical and applied aspects of analytical chemistry and analytical control, published since autumn 1997. Founder and publisher of the journal is the Ural Federal University named after the first President of Russia Boris Yeltsin (UrFU, Ekaterinburg).
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