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![Fig. 2. Effect of pH on absorbance of Mo(VI) – HMBATSC [Mo(VI)] = 5 x...](profile/Avvaru-Praveen-Kumar/publication/223998725/figure/fig1/AS:526570319691776@1502555555231/Effect-of-pH-on-absorbance-of-MoVI-HMBATSC-MoVI-5-x-10-5-M-HMBATSC-1-x_Q320.jpg)
![Fig. 3. Calibration plot [HMBATSC] = 1 x 10-3 M Wavelength = 385nm pH =1.5](profile/Avvaru-Praveen-Kumar/publication/223998725/figure/fig3/AS:526570320130048@1502555555370/Calibration-plot-HMBATSC-1-x-10-3-M-Wavelength-385nm-pH-15_Q320.jpg)
A rapid, simple, sensitive and selective spectrophotometric method is developed for the determination of molybdenum (VI) in aqueous dimethyl formamide (DMF). Molybdenum (VI) forms a yellow coloured complex with 2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone in the pH range 1.0-6.0. The complex shows maximum absorbance at 375nm and in the pH ran...
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... a 10ml standard flask containing 5ml of buffer of pH 1.5 and 1ml of (1x10 -2 M) HMBATSC solution, a suitable aliquot of the sample solution was added and the contents were diluted to 10ml with distilled water and its absorbance was measured at 385nm against the reagent blank. The amount of molybdenum present in these samples was computed from a pre-determined calibration plot and the results are presented in Table 2. Application to alloy steels A suitable aliquot of the sample solution was taken in a 10ml standard flask containing 5ml of buffer of pH 1.5, 1410 µg of Citrate ( to mask Cu) and 1ml of (1x10 -2 M) HMBATSC solution. ...
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2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone (HMBATSC) has been synthesized,
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A new spectrophotometric method has been developed for the determination of vanadium (IV) in
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soluble complex, [V(IV)–HMBATSC] in the pH range of 4.0...
2-Hydroxy-3-methoxy benzaldehyde thiosemicarbazone (HMBATSC) has been synthesized and its analytical applications are investigated. A rapid, simple, sensitive and selective spectrophotometric method is developed for the determination of palladium (II) in aqueous dimethyl formamide (DMF). Palladium (II) forrns a yellowish green coloured M2L3 complex...
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Citations
... All the above reasons push for a need to find an analytical method that could reasonably resolve the issues of skill and cost. Derivative spectrophotometry has become the method of choice for researchers, at beginner's level, who can now conveniently identify each component of complex mixtures [58], [59], [60]. It is an analytical technique which can qualitatively as well as quantitatively resolve the unresolved bands in spectra. ...
... The errors due to baseline shifts and tilts, medium turbidity, complex nature of mixtures, matrix background and light refraction are simultaneously eliminated [58]. The method is cost effective and has been validated for pharmaceutical formulations [31], [59], [61]. Moreover, it is simple, single step method (no extraction of vitamins) for vitamin B assay in food samples with no effect of interference from other molecules. ...
... Most of the extractive spectrophotometric methods developed for Mo(VI) are based on reactions with suitable colour producing reagents such as 2-(2 ' -furyl)-3-hydroxychromone in [1], quinolin-8-ol [2], thiocyanate and pyrogallol in MIBK [3], 2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone [4]. However, most of the existing methods suffer from limitations such as longer periods of time for phase separations, weak stability of coloured complexes and interferences from metal ions like tungsten, tin, antimony and anions and complexing agents like thiocyanate. ...
2,3,4-Trihydroxy Phenylethylidine Benzoic Acid Hydrazide (TPBH) as a photometric reagent for the extractive spectrophotometric determination of Molybdenum(VI) is presented in this paper. The reagent TPBH gave instantaneous and stable yellow colour with Molybdenum(VI) in the acidic pH range. The colour reaction in detail has been explored and the possibility of photometric determination of the micro amounts of molybdenum(VI) is established with necessary conditions. The system obeys Beer’s law in the range in the concentration range of 0.4-10 g/ml at 385 nm The optimal oncentration range is calculated from Ringbom plots are found to be 3-8 g/ml at 385 nm. The stoichiometry of the complex is established as 1:1 (M:L) by Job’s method of continuous variation and confirmed by mole ratio method. The stability constant, the standard deviation and the coefficient of variations are presented. The results of the prescribed procedure applied for the determination of the micro amounts of Mo(VI) in standard steel samples are presented.
... In this study, we are reporting a simple, sensitive, and selective second-order derivative simultaneous spectrophotometric method for Ru(III) and Pd(II) using 2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone (HMBATSC), which had been previously used for individual spectrophotometric determination of Pd (Sreevani et al. 2007), ...
A simple, sensitive, and selective second-order-derivative spectrophotometric method has been developed for the simultaneous determination of palladium(II) and ruthenium(III) using 2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone (HMBATSC) as a chromophoric reagent. The reagent (HMBATSC) reacts with Pd(II) and Ru(III) at pH 3.0, forming soluble yellowish green and dark brown species, respectively. Palladium and ruthenium present in the mixture were simultaneously determined without solving the simultaneous equations by measuring the second derivative amplitudes at 445nm and 385 nm, respectively. Further, the Beer's law was obeyed in the range 0.21-12.78 mu g mL(-1) and 0.25-13.42 mu g mL(-1) for Pd(II) and Ru(III), respectively. A large number of foreign ions did not interfere in the present method. The proposed method was successfully applied for the determination of palladium in hydrogenation catalysts and ruthenium in water samples.
Kinetic catalyzed effect of molybdenum on oxidation of complexing agent, 2,3,4-trihydroxy acetophenone phenylhydrozone (THAPPH) in view to develop a simple sensitive and selective kinetic spectropho-metric method for the determination of Mo(VI) was studied. The method sensitivity was calculated in terms of molar absorptive coefficient (16.91x10 4 L mo1-1 cm-1) and Sandell's sensitivity (0.642 μg cm-2), which explains that the method is more sensitive. The correlation coefficient of the color reaction is found to be 0.997, which indicates a better linearity between two variables. The developed method is more precise and accuracy, which is found by relative standard deviation (n=5), 0.32% and confidence limit, ± 0.002 with 0.0096 and 0.032μg cm-2 lower detection limit and lower quantity limit respectively. The color reaction forms 1:1(M:L)complex and its stability constant is calculated by Asumu's and Edmonds and Birnbaum's method. This developed method has also been applied for the determination of Mo(VI) from water samples and the validity of the method was checked by comparing the obtained results with AAS method and statically evaluation of obtained results in terms of student T-test and F-test. The present catalytic kinetic method is highly sensitive, selective and reproducible with an inexpensive for Mo(VI).
A very simple, ultra-sensitive and highly selective non-extractive spectrophotometric method for the determination of trace amounts of molybdenum(VI) in solution using benzoylacetone-benzoylhydrazone (Bzac-BH) has been developed. Bzac-BH reacts in a slightly acidic solution (0.0003–0.002 M H2SO4) with molybdenum(VI) to give an orange chelate which has an absorption maximum at 447 nm. The reaction is instantaneous and the absorbance remains stable for over 12 h. The average molar absorption co-efficient and Sandell's sensitivity were found to be 6.3 × 105 L mol−1 cm−1 and 15 ng cm−2 of molybdenum(VI), respectively. Linear calibration graphs were obtained for 0.05–2 mg L−1 of molybdenum(VI). The stoichiometric composition of the chelate is 1:1 (Mo:Bzac-BH). A large excess of over 50 cations, anions and complexing agents (such as chloride, phosphate, azide, thiosulfate, thiourea, SCN−, etc.) do not interfere with the determination. The developed method was successfully used in the determination of molybdenum levels in several Standard Reference Materials (alloys and steels) as well as in some environmental waters (inland and surface), biological samples (human blood and urine), soil samples, solutions containing both molybdenum(V) and molybdenum(VI) and complex synthetic mixtures. The method has high precision and accuracy (s = ±0.01 for 0.5 mg L−1).
A spectrophotometric method has been developed for the determination of ruthenium (Ru) (III) in an
aqueous dimethyl formamide using 2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone (HMBATC) as a
chromophoric reagent. The metal ion reacts with HMBATC forming a dark brown colored water soluble
complex in the acidic medium. The Ru-HMBATSC complex shows the absorption maximum at 375 nm.
However, at this wave length, the reagent shows considerable absorbance. At 390 nm, the complex shows large
absorbance while the reagent blank shows negligible absorbance. Hence the analytical studies were carried out
at 390 nm. Beer’s law is obeyed in the range of 0.50–8.10 g ml-1. The molar absorptivity and Sandell’s
sensitivity were 0.964 x 104 lit mol-1 cm-1 and 0.01 g cm-2 respectively. The interference effect of various
foreign ions has been studied. The complex has 1:1 [Ru(III)-HMBATSC] stoichiometry with a stability constant
of 5.8 x 107. The relative standard deviation of the method is found to be 1.56% (n=10). A first order derivative
spectroscopic method is developed for the determination of Ru (III), which is more sensitive than the zero order
method. The developed method has been employed for the determination of Ru (III) in synthetic mixtures and
water samples.
In present study, we summarized the analytical applications of thio- and phenylthiosemicarbazones in metal ions separation and determination from various samples by using spectrophotometer. We reviewed the analytical applications of thio and phenylthiosemicarbazones from 1991 to 2011. This two decades survey is very useful to the analytical chemists working on separation and determination of metal ions and biological activities of their complexes. In this article first we summarized the basic introduction and structural information of thio- and phenylthiosemicarbazones and then we reviewed their analytical applications in the separation and determination of metal ions from real samples, synthetic samples and alloy samples. Finally we discussed their biological activities. The literature survey reveals that the thio and phenyl thiosemicarbazones are promising chelating agents for the separation and determination of transitional metal ions. In addition to this the complexes formed by thio and phenylthiosemciarbazones with transitional metal ions are having biological activities.
Acetophenone 2',4'-dihydroxy semicarbazone (A24DHS) as a photometric reagent for the extractive spectrophotometric determination of Molybdenum (VI) is presented in this paper. The reagent A24DHS gave instantaneous and stable yellow colour with Molybdenum (VI) in the pH range 1.6 to 2.4. The system obeys Beer's law in the concentration range of 1.0 -g/mL to 8.0 -g/mL at 370 nm. The Limit of Detection (LOD) is calculated by using standard deviation of blank solution at confidence limit 98.3%, which is found to be 0.315 -g/mL. The stoichiometry of the complex is established as 1:3 (M:L) by Job's method of continuous variation and confirmed by mole ratio method. The standard deviation and the coefficient of variance are presented. The results of the prescribed procedure applied for the determination of the micro amounts of Mo (VI) in standard steel samples, alloys, pharmaceutical and synthetic samples are presented.
Several techniques have been proposed for treatment of spectrophotometric data, with the objective of extracting a largest amount of analytical information from spectra composed of unresolved bands. Undoubtedly, a major success was achieved by derivative treatment of the absorbance curves-plotting of the first or a higher order mathematical derivative of absorbance against wavelength (d A/d lambda). Derivative spectrophotometry has been applied to many chemical systems, such as pharmaceuticals, foods, cosmetics, and environmental samples. The instrumental development and analytical applications of derivative UV-vis regions absorption spectrophotometry produced in the last 5 years (since 2004) are reviewed.
