Hydroxyamidines as New Extracting Reagents for Spectrophotometric Determination of Cadmium with 4-(2-Pyridylazo)naphthol in Industrial Effluents, Coal, and Fly Ash

1993 ◽  
Vol 76 (3) ◽  
pp. 604-608 ◽  
Author(s):  
Sumon Chakravarty ◽  
Manas Kanti Deb ◽  
Rajendra Kumar Mishra

Abstract A simple, sensitive, and selective extractive spectrophotometric method for the determination of cadmium in trace quantities with N1-hydroxy-N1,N2- diphenylbenzamidine (HDPBA) and 4-(2-pyridylazo) naphthol (PAN) is described. The method is based on the extraction of cadmium with HDPBA into chloroform at pH 9.0 ± 0.2 and simultaneous spectrophotometric determination wiith PAN. The binary Cd(ll)-HDPBA complex extracted into chloroform has a molar absorptivity of 1.96 x 104L/ mol/cm at λmax 400 nm. The sensitivity of the yellow Cd(ll)-HDPBA complex was increased remarkably by the addition of PAN to the binary complex. With 6 different hydroxyamidines tested, the red-orange complex in chloroform exhibited maximum absorbance at 530-550 nm, with molar absorptivity values of 3.2-5.6 x 104L/mol/cm. The method adheres to Beer’s law up to 1.5 μg cadmium/mL organic phase. The detection limit of the method is 0.02 μg Cd/mL. Investigations of the effect of foreign ions revealed that the present method is free from matrix interference of most of the common ions (e.g., Fe(lll), Ni(ll), Cu(ll), Mn(ll), V(V), Co(ll), Al(lll), Cu(ll), Mg(ll), and Mo(VI)). The relative standard deviation for 10 repetitive analyses of the metal was 1.4%. The validity of the method was tested successfully with various environmental samples.

2021 ◽  
Vol 9 (2) ◽  
pp. 64-71
Author(s):  
Mykola Blazheyevskiy ◽  
◽  
Valeriy Moroz ◽  
Olena Mozgova ◽  
◽  
...  

The oxidative derivatization method using potassium hydrogenperoxomonosulfate for the indirect spectrophotometric determination of Fluphenazine hydrochloride is presented. Potassium hydrogenperoxomonosulfate is introduced as a derivatizing agent for Fluphenazine hydrochloride, yielding the sulfoxide. This reaction product was successfully used for the spectrophotometric determination of the Fluphenazine hydrochloride. The UV spectroscopic detection of the sulfoxide proved to be a more robust and sensitive method. The elaborated method allowed the determination of Fluphenazine hydrochloride in the concentration range of 0.2-30 µg mL-1. The molar absorptivity at 349 nm is 5.6×103 (dm3cm-1mol-1). The limit of quantification, LOQ (10S) is 0.24 µg/mL. A new spectrophotometric technique was developed and the possibility of quantitative determination of Fluphenazine hydrochloride in tablets 5.0 mg was demonstrated. The present method is precise, accurate and excipients did not interfere. RSD for Fluphenazine Hydrochloride 5.0 mg tablets was 1.37 %.


1993 ◽  
Vol 76 (3) ◽  
pp. 601-603 ◽  
Author(s):  
A A Al-Warthan ◽  
S S Al-Showiman ◽  
S A Al-Tamrah ◽  
A A BaOsman

Abstract The formation of a red complex between boron and the quinalizarin reagent was investigated and used as the basis for a simple and sensitive spectrophotometric method for boron in date cultivars. At 620 nm, the absorbance was linear (r= 0.999) over the 0.25-2.5 μg/mL concentration range. The molar absorptivity was found to be 2.23 x 103mol-1cm-1 and the relative standard deviation for 10 replicates (1.0 μg/mL) was 0.97%.


2008 ◽  
Vol 59 (1) ◽  
pp. 3-7
Author(s):  
Aurora Reiss ◽  
Mihaela Mureseanu ◽  
Nicolae Muresan

5-Hydroxy-6-mercapto-benzo [a] phenazine (HMBP) is proposed as a sensitive and selective analytical reagent for the extractive spectrophotometric determination of copper (II). Copper reacts with HMBP to give a dark red complex which is soluble in chloroform. The composition of the CuII � HMBP complex is established as 1:2 by Job�s continuous variation method and molar ratio method. The instability constant of the complex calculated by Job�s relation for nonisomolar series is 4.65 . 10-9, at room temperature. The CuII-HMBP complex in chlorophorm shows a maximum absorbance at 495 nm, with molar absorptivity and Sandell�s sensitivity values of 7.39 . 103dm3 mol-1 cm-1 and 0.012 mg cm-2, respectively. Beer�s law is obeyed in the concentration range 0.67 - 26.90 mg mL-1 and the detection limit is 0.59 mg mL-1. A repetition of the method is checked by finding the relative standard deviation (RSD) at 1.00 mg mL-1 CuII of 0.6%. The method is successfully employed for the determination of copper (II) in environmental samples. The reliability of the method is assured by analysing the standard alloys and by inter-comparison of experimental values, using an atomic absorption spectrometer.


2020 ◽  
Vol 33 (1) ◽  
pp. 18-23
Author(s):  
Harshita Sharma ◽  
Anushree Saha ◽  
Chhaya Bhatt ◽  
Kalpana Wani ◽  
Ajay Kumar Sahu ◽  
...  

The proposed method is based on flotation–dissolution an easy, impressible, extractive spectrophotometric determination, explained for easy investigation of the organophosphate pesticide phorate (O,O-diethyl S-[ethylthiomethyl] phosphorodithioate) on trace levels. A molybdophospho complex is generated when prorate is treated with ammonium molybdate in acidic medium. As an ion associate complex with methylene blue the complex is present in between of the water and organic layers which is extracted and then dissolved with acetone. The greenish blue complex produced show absorption maxima at 660 nm. Beer’s law range is found to be 0.5 to 16 µg per 10 ml for phorate. The molar absorptivity is 0.989×103 L mol-1 cm-1 and sandell’s sensitivity is 1.00×10-5 µg cm-2. Also calculated the standard deviation and relative standard deviation for the above method were ±0.006 and 1.95% respectively. The method has been applied and checked for the determination of phorate in water, soil and vegetables.


2015 ◽  
Vol 69 (4) ◽  
Author(s):  
Teodora S. Stefanova ◽  
Kiril K. Simitchiev ◽  
Kiril B. Gavazov

AbstractLiquid-liquid extraction (LLE) and cloud point extraction (CPE) of vanadium(V) ternary complexes with 4-(2-pyridylazo)resorcinol (PAR) and 2,3,5-triphenyl-2H-tetrazolum chloride (TTC) were investigated. The optimal conditions for vanadium extraction and spectrophotometric determination were identified. The composition (V : PAR : TTC) of the extracted species was 1 : 2 : 3 (optimal conditions; LLE), 2 : 2 : 2 (low reagents concentrations; LLE), 1 : 1 : 1 (short heating time; CPE), and 1 : 1 : 1 + 1 : 1 : 0 (optimal extraction conditions; CPE). LLE, performed in the presence of 1,2-diaminocyclohexane-N,N,N’,N’-tetraacetic acid and NH4F as masking agents, afforded the sensitive, selective, precise, and inexpensive spectrophotometric determination of vanadium. The absorption maximum, molar absorptivity, limit of detection, and linear working range were 559 nm, 1.95 × 105 dm3 mol−1 cm−1, 0.7 ng cm−3, and 2.2-510 ng cm−3, respectively. The procedure thus developed was applied to the analysis of drinking waters and steels. The relative standard deviations for V(V) determination were below 9.4 % (4-6 × 10−7 mass %; water samples) and 2.12 % (1-3 mass %; steel samples).


2017 ◽  
Vol 9 (4) ◽  
pp. 49 ◽  
Author(s):  
Lazeeza Sattar Omer ◽  
Rasul Jameel Ali

Simple, selective and highly detectable spectrophotometric method has been developed and validated for the determination of Lidocaine hydrochloride in standard and commercial solutions .The method is based on the formation of a soluble colored Lidocaine hydrochloride-eriochrome black T ion-pair complex at pH 1.80. The colored complex was extracted quantitatively into chloroform and measured at 508 nm. Beer’s law was obeyed in the concentration range of 0.10-10 mg L -1 with molar absorptivity of 2.3623 x104 L mol-1 cm-1.The limits of detection and quantification were 0.024 mg L -1, and 0.100 mg L -1 respectively. Using Job’s continuous variations method, the stoichiometry of the ion-pair complex was found to be 1:1. Intra-day accuracy and precision of the method were estimated with a relative error (0.57%), and the relative standard deviation (0.25-1.23). This developed method has been successfully employed to determine concentration of Lidocaine hydrochloride in injection and spray without interference by the common co-formulated substances.The numerical results obtained using both proposed and official methods were in concordance with each other.


2021 ◽  
Vol 30 (1) ◽  
pp. 60-65
Author(s):  
Mamta Nirmal ◽  
Prashant Mundeja ◽  
Kalpana Wan ◽  
Vindhiya Patel ◽  
Raisa Khatoon ◽  
...  

Simple and sensitive spectrophotometric scheme was described for the determination of fenvalerate in environmental samples. The scheme was based on the hydrolysis of 1 N of 5 mL NaOH to form cyanohydrin. The cyanohydrin is reacted with bromine and pyridine to form glutaconic aldehyde, which is then coupled with p-Dimethylaminobenzaldehyde to give yellow dye having maximum absorbance at 440 nm. Beer’s law is obeyed over the concentration range of 0.6- 6.2 µg in a nal solution volume of 25 mL. The molar absorptivity of the colored system is 3.84×104 L mol-1cm-1 and Sandell’s sensitivity is 2.4×10-3 µg cm-2. The reproducibility assessed by carrying out seven days replicate analysis of a solution containing 0.6 µg of fenvalerate in a nal solution volume of 25 mL. The standard deviation and relative standard deviation for the absorbance value were found to be ± 3.4×10-3 and 1.5% respectively. The proposed scheme is sensitive and free from the interference of other toxicants. The analytical parameters were optimized and the scheme was applied to the determination of fenvalerate in environmental samples.


2001 ◽  
Vol 84 (2) ◽  
pp. 399-406 ◽  
Author(s):  
Khageshwar Singh Patel ◽  
Aditya Shukla ◽  
Neeta Agarwal ◽  
Peter Hoffmann

Abstract A new, sensitive, and selective method is described for the spectrophotometric determination of Ta(V). The method is based on the extraction of the Ta(V)–F−–CV+ complex (CV+ = crystal violet cation) with a benzene solution of imidoyl derivatives (ID), i.e., N,N′-diphenylbenzamidine (DPBA), N-hydroxy- N,N′-diphenylbenzamidine, and N-(2,5-dimethyl)phenyl-p-tolylimidoylphenylhydrazine, from sulfuric acid solution; DPBA was selected for detailed study. The molar absorptivities of the Ta(V)–F−–CV+–ID complexes in the benzene solution were in the range of (1.00–1.65) × 105 L/mol·cm at 600 nm. The limit of detection was 7 ng Ta/mL (which had an absorbance greater than that of the blank + 3 standard deviations). The optimization of the analytical variables, the composition of the complex, and the effect of diverse ions in the determination of Ta are discussed. The present method was applied to the determination of Ta in environmental samples, i.e., soil, sediment, minerals, and alloys.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Rameshwar Dass ◽  
Jitander K. Kapoor ◽  
Sunita Gambhir

An extractive spectrophotometric method has been developed for microdetermination of molybdenum. At room temperature Mo(VI) was reduced to Mo(V) in 2 M H2SO4using ascorbic acid as a reductant. The Mo(V) formed a yellow-coloured (1 : 2) complex with 6-chloro-3-hydroxy-2-(3′-hydroxyphenyl)-4-oxo-4H-1-benzopyran (CHHB). The complex was quantitatively extracted into toluene and absorbed maximum atλmax404 nm. Beer’s law was obeyed over the concentration range of 2.31 μg Mo ml−1with a molar absorptivity and Sandell's sensitivity of5.62×104 L mol−1 cm−1and 0.0016 μg Mo cm−2, respectively. The relative standard deviation was 0.0025 (in absorbance units) for 10 replicate determinations of 1 μg Mo ml−1. The method was free from the interference of large number of analytically important elements. Molybdenum has been determined satisfactorily in different technical, synthetic, and environmental samples with improved accuracy and precision.


2006 ◽  
Vol 129 (1-3) ◽  
pp. 271-276 ◽  
Author(s):  
K. Suresh Kumar ◽  
K. Suvardhan ◽  
D. Rekha ◽  
K. Kiran ◽  
G. Chalapathi Rao ◽  
...  

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