Multicomponent Spectrophotometric Analysis of Metal Ions Based on Simultaneous or Consecutive Application of Several Reagents

1994 ◽  
Vol 59 (9) ◽  
pp. 1951-1963
Author(s):  
Jiří Perůtka ◽  
Josef Havel ◽  
Luděk Jančář

This paper deals with nonconventional approaches to multicomponent spectrophotometric analysis consisting of (i) simultaneous or consecutive addition of several nonselective reagents in the multicomponent determination of metal ions, and (ii) the use of absorbance data which have been measured at different pH values or in different experimental conditions and subsequently combined into a single data set, evaluated by the partial least squares method. The following multicomponent mixtures of metal ions with reagents were examined: Co2+ and Fe3+ with nitroso-R-salt and 1,10-phenanthroline; Co2+, Cu2+ and Fe3+ with nitroso-R-salt and zincon; Co2+, Cu2+ and Zn2+ with nitroso- R-salt and zincon; and Cu2+, Zn2+ and Ni2+ with zincon and PAR. The average relative error of determination was 2% (two metal ions) and 5% (three metal ions). Cu2+, Zn2+ and Ni2+ were also quantitated in ALPAKA alloy with relative errors of 4 - 9%.

Author(s):  
LIPSA SAMAL ◽  
AMARESH PRUSTY

Objective: The aim of the present work was to develop and validate a simple UV spectroscopic method for the determination of duloxetine, which is a thiophene derivative and a selective neurotransmitter reuptake inhibitor for serotonin, norepinephrine, and to lesser degree dopamine. Methods: The UV Spectrophotometric analysis was performed using Shimadzu UV-1800 and Shimadzu UV-1700 spectrophotometer by using solvent system acetonitrile and water in the ratio of 8:2. Detection was performed at a wavelength of 290 nm. Method validation was carried out according to ICH Q2R1 guidelines by taking the parameters linearity, accuracy, precision, ruggedness, and robustness, LOD and LOQ. Results: The UV Spectrophotometric method was found linear in the range of 10-50 μg/ml. The method was rugged and robust with % relative standard deviation less than 2. The extraction recoveries were found to be higher than 99% in all experimental conditions. Conclusion: Based upon the performance characteristics, the proposed method was found accurate, precise and rapid and suitable for the determination of Duloxetine for routine analysis.


2013 ◽  
Vol 807-809 ◽  
pp. 456-460
Author(s):  
Xin Rong Wen ◽  
Chang Qing Tu

The paper presents a novel method for the separation/enrichment of trace Cu2+ using microcrystalline phenolphthalein loaded with cupferron (Cup) prior to the determination by spectrophoto- metry. The effects of different parameters,such as the dosages of phenolphthalein and Cup and acidity on the enrichment yield of Cu2+ have been investigated to select the experimental conditions. The possible enrichment mechanism of Cu2+ was discussed.The results showed that under the optimum conditions, Cu2+ could be quantificationally adsorbed on the surface of microcrystalline phenolphthalein in the form of the chelate precipitate of Cu (Cup)2 ,while Ni2+,Zn2+,Mn2+,Fe2+ and Al3+ could not be adsorbed at all.Therefore,Cu2+ was completely separated from the above metal ions in the solution. The quantitative separation/enrichment and determination of Cu2+ in various environmental water samples was performed, and the results agreed well with those obtained by FAAS method.


2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Kai Sun ◽  
Qingzhu Liu ◽  
Rui Zhu ◽  
Qi Liu ◽  
Shunyao Li ◽  
...  

Certain nano-scale metal oxides exhibiting the intrinsic enzyme-like reactivity had been used for environment monitoring. Herein, we evaluated the oxidase-mimicking activity of environmentally relevant nano-MnO2 and its sensitivity to the presence of metal ions, and particularly, the use of MnO2 nanozyme to potentially detect Cu2+, Zn2+, Mn2+, and Fe2+ in water. The results indicated the oxidase-like activity of nano-MnO2 at acidic pH-driven oxidation of 2,6-dimethoxyphenol (2,6-DMP) via a single-electron transfer process, leading to the formation of a yellow product. Notably, the presence of Cu2+ and Mn2+ heightened the oxidase-mimicking activity of nano-MnO2 at 25°C and pH 3.8, showing that Cu2+ and Mn2+ could modify the reactive sites of nano-MnO2 surface to ameliorate its catalytic activity, while the activity of MnO2 nanozyme in systems with Zn2+ and Fe2+ was impeded probably because of the strong affinity of Zn2+ and Fe2+ toward nano-MnO2 surface. Based on these effects, we designed a procedure to use MnO2 nanozyme to, respectively, detect Cu2+, Zn2+, Mn2+, and Fe2+ in the real water samples. MnO2 nanozyme-based detecting systems achieved high accuracy (relative errors: 2.2–26.1%) and recovery (93.0–124.0%) for detection of the four metal ions, respectively. Such cost-effective detecting systems may provide a potential application for quantitative determination of metal ions in real water environmental samples.


Author(s):  
Ling Gao ◽  
Shouxin Ren

This paper presented a novel method named wavelet packet transform-based partial least squares method (WPTPLS) for simultaneous spectrophotometric determination ofα-naphthylamine, p-nitroaniline, and benzidine. Wavelet packet representations of signals provided a local time-frequency description and separation ability between information and noise. The quality of the noise removal can be improved by using best-basis algorithm and thresholding operation. Partial least squares (PLS) method uses both the response and concentration information to enhance its ability of prediction. In this case, by optimization, wavelet function and decomposition level for WPTPLS method were selected as Db16 and 3, respectively. The relative standard errors of prediction (RSEP) for all components with WPTPLS and PLS were 2.23% and 2.71%, respectively. Experimental results showed WPTPLS method to be successful and better than PLS.


2000 ◽  
Vol 663 ◽  
Author(s):  
C. Ekberg ◽  
P. Brown ◽  
J. Comarmond ◽  
Y. Albinsson

ABSTRACTThe stability constants of the hydroxide complexes of zirconium(IV) and uranium(IV) have been measured at 15, 25 and 35°C [in 1.0 mol dm−3 (Na, H)ClO4] using potentiometry. For zirconium(IV), the results indicate the presence of Zr(OH)3+ and the polymeric species Zr3(OH)48+ and Zr4(OH)88+ whereas the results for uranium(IV) indicate the presence of U(OH)3+ and the polymeric species U4(OH)124+. The hydrolysis of both metal ions was studied at three temperatures allowing the determination of ΔH° and ΔS° of reaction for each species. The results were compared with previous results determined for thorium(IV) under the same experimental conditions to ascertain whether thorium should be used as an analogue for other tetravalent metal ions in safety assessment studies of nuclear repositories.


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