scholarly journals A Rapid Spectrophotometric Method for the Determination of Trace Level Lead Using 1,5-Diphenylthiocarbazone in Aqueous Micellar Solutions

2007 ◽  
Vol 23 (2) ◽  
pp. 193-199 ◽  
Author(s):  
Humaira KHAN ◽  
M. Jamaluddin AHMED ◽  
M. Iqbal BHANGER
2006 ◽  
Vol 20 (5-6) ◽  
pp. 285-297 ◽  
Author(s):  
Humaira Khan ◽  
M. Jamaluddin Ahmed ◽  
M. Iqbal Bhanger

A very simple, ultra-sensitive and fairly selective new spectrophotometric method has been developed for the rapid determination of lead(II) at ultra-trace level using 1,5-diphenylthiocarbazone (dithizone) in presence of aqueous micellar solutions. The proposed method enabled the determination of lead down to µg l−1in human blood and urine in aqueous media without resource of any “clean-up” step. The most remarkable point of this method is that the presence of micellar system avoids the previous steps of solvent extraction and reduces the cost, toxicity while enhancing the sensitivity, selectivity and the molar absorptivity. The complex formation of lead in blood with dithizone was completed within a minute at room temperature and the absorbance remains stable for 24 h. The average molar absorption coefficient and Sandell's sensitivity were found to be 3.99×105l mol−1 cm−1and 30 ng cm−2of Pb, respectively. Linear calibration graphs were obtained for 0.06–60 mg l−1of PbII; the stoichiometric composition of the chelate is 1:2 (Pb:dithizone). The interference from over 60 cations, anions and complexing agents has been studied at 1 mg l−1of PbII. The method was successfully used in the determination of lead in several biological samples (human blood and urine and bovine liver), solution containing both lead(II) and lead(IV) and complex synthetic mixtures. The results of biological analyses by the spectrophotometric method were in excellent agreement with those obtained by AAS. The results of lead concentration in biological samples were varied with age, sex and place which have been discussed.


2008 ◽  
Vol 3 ◽  
pp. ACI.S977 ◽  
Author(s):  
Rubina Soomro ◽  
M. Jamaluddin Ahmed ◽  
Najma Memon ◽  
Humaira Khan

A simple high sensitive, selective, and rapid spectrophotometric method for the determination of trace gold based on the rapid reaction of gold(III) with bis(salicylaldehyde)orthophenylenediamine (BSOPD) in aqueous and micellar media has been developed. BSOPD reacts with gold(III) in slightly acidic solution to form a 1:1 brownish-yellow complex, which has an maximum absorption peak at 490 nm in both aqueous and micellar media. The most remarkable point of this method is that the molar absorptivities of the gold-BSOPD complex form in the presence of the nonionic TritonX-100 surfactant are almost a 10 times higher than the value observed in the aqueous solution, resulting in an increase in the sensitivity and selectivity of the method. The apparent molar absorptivities were found to be 2.3 x 10 4 L mol-1 cm-1 and 2.5 x 10 5 L mol-1 cm-1 in aqueous and micellar media, respectively. The reaction is instantaneous and the maximum absorbance was obtained after 10 min at 490 nm and remains constant for over 24 h at room temperature. The linear calibration graphs were obtained for 0.1 -30 mg L-1 and 0.01 -30 mg L-1 of gold(III) in aqueous and surfactant media, respectively. The interference from over 50 cations, anions and complexing agents has been studied at 1 mg L-1 of Au(III); most metal ions can be tolerated in considerable amounts in aqueous micellar solutions. The Sandell's sensitivity, the limit of detection and relative standard deviation (n = 9) were found to be 5 ng cm-2, 1 ng mL-1 and 2%, respectively in aqueous micellar solutions. Its sensitivity and selectivity are remarkably higher than that of other reagents in the literature. The proposed method was successfully used in the determination of gold in several standard reference materials (alloys and steels), environmental water samples (potable and polluted), and biological samples (blood and urine), geological, soil and complex synthetic mixtures. The results obtained agree well with those samples analyzed by atomic absorption spectrophotometry (AAS).


2018 ◽  
pp. 54-59
Author(s):  
A.R. Guliyeva ◽  
◽  
A.M. Maharramov ◽  
F.M. Chiragov ◽  
P.R. Mammadov ◽  
...  

2012 ◽  
Vol 11 (1) ◽  
pp. 15-30
Author(s):  
Anitha Varghese ◽  
A M A Khadar

A simple, selective and sensitive spectrophotometric method has been developed for the determination of trace amounts of thorium using a newly synthesised reagent diacetylmonoximep-hydroxybenzoylhydrazone (DMPHBH) in the presence of Triton X-100. The molar absorptivity and Sandell’s sensitivity of the coloured species at pH 4.4 were found to be 4.20 x 104 L mol-1 cm-1 and 5.5 ng cm-2, respectively. Beer’s law is obeyed in the range 0.35 -3.8 mg mL-1 of thorium(IV) at 410 nm. The stoichiometry of the complex was found to be 1:2 (Th(IV): DMPHBH). A highly selective first order derivative spectrophotometric method for the determination of thorium in the presence of uranium is also reported. The detection limit and quantitation limit of first order derivative spectrophotometry were found to be 0.03 and 0.11 mg mL-1, respectively. The developed procedure has been successfully applied for the trace level determination of thorium in rock samples and synthetic mixtures.


Molekul ◽  
2006 ◽  
Vol 1 (1) ◽  
pp. 45
Author(s):  
Irmanto Irmanto ◽  
Suyata Suyata

A spectrophotometric method for the determination of oxalic acid has been developed, based on its catalytic effect on the redox reaction between methylene blue and sulphide, measured at the maximum absorption wavelength of 664 nm. Under the optimum conditions of 3 mL of 31 % formaldehyde; 0.8 mL of 0,067 M EDTA - Triethanolamine; 1.2 mL of 0,010 M sulphide; 2 mL of 0,0010 % methylene blue at 20 oC for 1 minute a detection limit of 0,43 mg/mL for oxalic acid determination was obtained. This method can be applied to determination of trace level of oxalic acid.


2008 ◽  
Vol 7 (1) ◽  
pp. 13-25
Author(s):  
Anitha Varghese ◽  
A. M. A. Khadar

A simple, selective and sensitive spectrophotometric method has been developed for the determination of trace amounts of Vanadium(V) in acetic acid medium using a newly synthesized reagent acetoacetanilide salicyloylhydrazone (AASH). The molar absorptivity and Sandell's sensitivity of the coloured species were found to be 1.20 x 104 L mol-1cm-1 and 4.2 ng cm-2 respectively. Beer's law is obeyed in the range 0.3 -3.0μ.g mL-1 of vanadium (V) at 405 nm. The stochiometry of the complex was found to be 1:1 (V (V): AASH). A highly selective first order derivative spectrophotometric method for the determination of vanadium is also reported. A calibration graph was derived by measuring first derivative amplitudes at 430 nm (trough depth). The metal ions which are normally associated with vanadium in minerals and alloys do not interfere. The developed procedure has been successfully applied for the trace level determination of vanadium in steels, minerals and soil samples.


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