Speciation determination of chromium(III) and (VI) using preconcentration cloud point extraction with flame atomic absorption spectrometry (FAAS).

bis-[2-Hydroxy-1-naphthaldehyde] thiourea was synthesized and preconcentration cloud point extraction (CPE) for speciation determination of chromium(III) and (VI) in various environmental samples with flame atomic absorption spectrometry (FAAS) has been developed. Chromium(III) complexes with bis-[2-hydroxynaphthaldehyde] thiourea is subsequently entrapped in the surfactant micelles. After complexation of chromium(III) with reagent, the analyte was quantitatively extracted to the surfactant-rich phase in the non-ionic surfactant Triton X-100 after centrifugation. The effect of pH, concentration of chelating agent, surfactant, equilibration temperature and time on CPE was studied. The relative standard deviation was 2.13% and the limits of detection were around 0.18 microg L(-1).

WITHDRAWN: Copper(II) preconcentration on Amberlite XAD-2010 loaded microorganisms prior to its spectrophotometric determination.

This article has been withdrawn consistent with Elsevier Policy on Article Withdrawal (http://www.elsevier.com/locate/withdrawalpolicy). The Publisher apologizes for any inconvenience this may cause.

Preconcentration and solid phase extraction method for the determination of Co, Cu, Ni, Zn and Cd in environmental and biological samples using activated carbon by FAAS.

2-{[1-(2-Hydroxynaphthyl) methylidene] amino} benzoic acid (HNMABA) was synthesized for solid phase extraction (SPE) to the determination of Co, Cu, Ni, Zn and Cd in environmental and biological samples by flame atomic absorption spectrophotometry (FAAS). These metals were sorbed as HNMABA complexes on activated carbon (AC) at the pH range of 5.0+/-0.2 and eluted with 6 ml of 1M HNO3 in acetone. The effects of sample volume, eluent volume and recovery have been investigated to enhance the sensitivity and selectivity of proposed method. The effect of interferences on the sorption of metal ions was studied. The concentration of the metal ions detected after preconcentration was in agreement with the added amount. The detection limits for the metals studied were in the range of 0.75-3.82 microg ml(-1). The proposed system produced satisfactory results for the determination of Co, Cu, Ni, Zn and Cd metals in environmental and biological samples.

Solid phase extraction method for the determination of lead, nickel, copper and manganese by flame atomic absorption spectrometry using sodium bispiperdine-1,1'-carbotetrathioate (Na-BPCTT) in water samples.

A novel column solid phase extraction procedure was developed for the determination of lead, nickel, copper and manganese in various water samples by flame atomic absorption spectrometry (FAAS) after preconcentration on sodium bispiperdine-1,1'-carbotetrathioate (Na-BPCTT) supported by Amberlite XAD-7. The sorbed element was subsequently eluted with 1M nitric acid and the acid eluates are analysed by Flame atomic absorption spectrometry (FAAS). Various parameters such as pH, amount of adsorbent, eluent type and volume, flow-rate of the sample solution, volume of the sample solution and matrix interference effect on the retention of the metal ions have been studied. The optimum pH for the sorption of above mentioned metal ions was about 6.0+/-0.2. The loading capacity of adsorbent for Pb, Cu, Ni and Mn were found to 28, 26, 22 and 20x10(-6) g/mL, respectively. The recoveries of lead, copper, nickel and manganese under optimum conditions were found to be 96.7-99.2 at the 95% confident level. The limit of detection was 3.0, 3.2, 2.8 and 3.6x10(-6) g/mL for lead, copper, nickel and manganese, respectively by applying a preconcentration factor 50. The proposed enrichment method was applied for metal ions in various water samples. The results were obtained are good agreement with reported method.

Facile and sensitive spectrophotometric determination of vanadium in various samples.

Novel reactions were developed for facile, sensitive and selective rapid spectrophotometric determination of trace amounts of vanadium(V) in various samples. The methods were based on the interactions of 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) with N-(1-naphthyl)ethylenediamine dihydrochloride (NEDA) in the presence of vanadium to give blue colored derivative or on oxidation of dopamine hydrochloride (DPH) by vanadium in acidic medium and coupling with MBTH to yield pink color derivative. The blue color derivative having an absorbance maximum at 595nm was stable for 9 days and the pink color derivative with λ(max) 526nm for 5 days. Beer's law is obeyed for vanadium in the concentration range 0.05-6.0µgml(-1) (blue color derivative) and 0.06-7.0µgml(-1) (pink color derivative), respectively. The optimum reaction conditions and other important analytical parameters were established. Interference due to various non-target ions was also investigated. The proposed methods were applied to the analysis of vanadium(V) in environmental, biological, pharmaceutical and steel samples. The performance of proposed method was evaluated in terms of Student's t-test and variance ratio F-test that indicates the significance of proposed method over reported method.

RETRACTED: Development of novel reactions for the simple and sensitive spectrophotometric determination of vanadium in various samples.

This article has been retracted at the request of the Editors-in-Chief. Please see Elsevier Policy on Article Withdrawal (http://www.elsevier.com/locate/withdrawalpolicy). Reason: Considerable concern was raised about the research purportedly conducted at Sri Venkateswara University, India with the alleged involvement of Professor P. Chiranjeevi. Questions were raised as to the volume of publications, the actual capacity (equipment, orientation and chemicals) of the laboratory in which Professor Chiranjeevi worked, the validity of certain of the research data identified in the articles, the fact that a number of papers appear to have been plagiarized from other previously published papers, and some aspects of authorship. Professor Chiranjeevi was given the opportunity to respond to these allegations. Thereafter, a committee was constituted by the University to look into these allegations. Based on the enquiry committee report, we have been informed by the head of the Department of Chemistry at Sri Venkateswara University that the university authorities have taken disciplinary action against ProfessorChiranjeevi, as the university considers that there are grounds for such action. Therefore, based on the results of this investigation, the Editors-in-Chief are retracting this article.

Spectrophotometric determination of V(V) in environmental, biological, pharmaceutical and alloy samples by novel oxidative coupling reactions.

A Novel, rapid, sensitive and selective reactions are developed for spectrophotometric determination of trace amounts of vanadium (V) in environmental, biological, pharmaceutical and alloy samples was studied. The methods were based on interactions of 4-bromophenyl hydrazine (4-BPH) with N-(1-naphthyl ethylenediamine dihydrochloride (NEDA) in the presence of vanadium in acidic medium (acetate buffer of pH 3.0) to give violet colored derivative or on the oxidation of 4-bromophenyl hydrazine by vanadium in basic medium and coupling with chromotropic acid (CA) to yield red color derivative. The violet color derivative having an absorbance maximum at 570nm which is stable for 7 days and the red derivative with lambda(max) 495nm for 5 days. Beer's law was obeyed for vanadium in the concentration range of 0.5-6.0microgml(-1) (violet derivative) and 0.6-7.0microgml(-1) (red derivative), respectively. The optimum reaction conditions and other important analytical parameters were established to enhance the sensitivity of the proposed methods. Interference due to various non-target ions was also investigated. The proposed methods were applied to the analysis of vanadium (V) in environmental, biological, pharmaceutical and steel samples. The performance of proposed methods were evaluated in terms of Student's t-test and Variance ratio F-test that indicates the significance of proposed methods over reported method.

Development of simple and sensitive spectrophotometric method for the determination of bendiocarb in its formulations and environmental samples.

Facile, selective and sensitive spectrophotometric method has been developed for the determination of bendiocarb in its insecticidal formulations, fortified water, food grains, agriculture wastewater and agriculture soil samples with prepared reagents. The method was based on alkaline hydrolysis of the bendiocarb pesticide, and the resultant hydrolysis product of bendiocarb was coupled with 2,6-dibromo-4-methylaniline to give a yellow color product with lambda max of 457 nm or coupling with 2, 6-dibromo-4-nitroaniline to produce a red colored product with lambda max of 474 nm or coupling with 2, 4, 6-tribromoaniline to form orange red colored product has a lambda max of 465 nm. Under optimal conditions, Beer's law range for 2, 6-dibromo-4-methylaniline (DBMA) was found to be 0.6-14.0 microg mL (-1), 0.8-10.0 microg mL (-1) for 2, 6-dibromo-4-nitroaniline (DBNA) and 0.4-10.0 microg mL (-1) for 2, 4, 6-tribromoaniline (TBA). The molar absorptivity of the color systems were found to be 4.126 x 10(4) l mol (-1) cm (-1) for DBMA, 3.254 x 10(4) l mol (-1) cm (-1) for DBNA and 2.812 x 10(4) l mol (-1) cm (-1) for TBA. Sandell's of the color reactions are 0.018 microg cm (-2)(DBMA), 0.052 microg cm (-2)(DBNA) and 0.065 microg cm (-2) (TBA) respectively. The effect of the non-target species on the determination of bendiocarb was studied. The formation of colored derivatives with the coupling agents is instantaneous and stable for 18 h, 30 h, and 12 h. Performance of the proposed methods were compared statistically in terms Student's F and t-tests with the reported methods.

Facile and sensitive spectrophotometric determination of carbosulfan in formulations and environmental samples.

Facile, selective and sensitive spectrophotometric method has been developed for the determination of carbosulfan in insecticidal formulations, fortified water, food grains, agriculture wastewater and soil samples with newly synthesized reagents. The method was based on acid and alkaline hydrolysis of the carbosulfan pesticide, and the resultant hydrolysis product of carbosulfan was coupled with 2,6-dibromo-4-methylaniline to give a yellow color product with lambda(max) of 464 nm or interaction with 2,6-dibromo-4-nitroaniline to produce yellow colored product with lambda(max) of 408 nm or coupling with 2,4,6-tribromoaniline to form red colored product has a lambda(max) of 471 nm. Under optimal conditions, Beer's law range for 2,6-dibromo-4-methylaniline (DBMA) was found to be 0.2-12.0 microg ml(-1), 0.6-16.0 microg ml(-1) for 2,6-dibromo-4-nitroaniline (DBNA) and 0.4-15.0 microg ml(-1) for 2,4,6-tribromoaniline (TBA). The molar absorptivity of the color systems were found to be 3.112 x 10(4) l mol(-1) cm(-1) for DBMA, 3.214 x 10(4) l mol(-1) cm(-1) for DBNA and 3.881 x 10(4) l mol(-1) cm(-1) for TBA. Sandell's of the color reactions are 0.013 microg cm(-2) (DBMA), 0.012 microg cm(-2) (DBNA) and 0.011 microg cm(-2) (TBA) respectively. The effect of the non-target species on the determination of carbosulfan was studied to enhance the selectivity of the proposed methods. The formation of colored derivatives with the coupling agents is instantaneous and stable for 28, 30, and 26 h. Performance of the proposed methods were compared statistically in terms Student's F and t-tests with the reported methods.

Preconcentration technique for the determination of trace elements in natural water samples by ICP-AES.

A procedure was developed for the determination of Cd, Cu, Zn, Co, Ni, Mn, Pb and Mo in water samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) after preconcentration on a morpholine dithiocarbamate (mor-DTC) supported by bagasse (Saccharam aphisinaram). The sorbed elements were subsequently eluted with 4,M HNO3 and the acid eluates were analysed by ICP-AES. The influence of various parameters such as pH, flow rate of sample, eluent concentration, volume of the sample and volume of eluent were investigated to enhance the sensitivity of the present method. A 20,mL disposable syringe served as preconcentration column. Under the optimal conditions Cd, Cu, Zn, Co, Ni, Mn, Pb and Mo in aqueous sample was concentrated about 100-fold. The sorption recoveries of elements were higher than 99.6%. The method is also applied for the analysis of natural and spiked water samples.

Simple, selective and sensitive spectrophotometric determination of fenitrothion using novel chromogenic reagent.

A facile, rapid and sensitive spectrophotometric method was developed for the determination of fenitrothion in its formulations, water, food grain and agriculture soil samples with newly synthesised reagent. The method was based on the alkaline hydrolysis of fenitrothion pesticide and resultant hydrolysed product of fenitrothion was coupled with diazotised 4,4'-methylene-bis-(p-amino-3'-hydroxybenzanilide) in basic medium to give orange coloured product having lambdamax 480 nm. The formation of coloured derivatives with the coupling agent is instantaneous and stable for 48 h. Beer's law was obeyed in the concentration range of 0.1-19.0 microg ml(-1). The proposed method is sensitive, easy to operate and permitted the determination of fenitrothion with a detection limits of 0.085 microg ml(-1). The experimental results indicate that the procedure can eliminate the fundamental interferences caused by other pesticides and non-target ions, which made these methods more sensitive and selective. The method was applicable to the determination of fenitrothion residue in water, food grain and soil samples up to ng level.

Cloud point extraction of palladium in water samples and alloy mixtures using new synthesized reagent with flame atomic absorption spectrometry (FAAS).

The present paper outlines novel, simple and sensitive method for the determination of palladium by flame atomic absorption spectrometry (FAAS) after separation and preconcentration by cloud point extraction (CPE). The cloud point methodology was successfully applied for palladium determination by using new reagent 4-(2-naphthalenyl)thiozol-2yl azo chromotropic acid (NTACA) and hydrophobic ligand Triton X-114 as chelating agent and nonionic surfactant respectively in the water samples and alloys. The following parameters such as pH, concentration of the reagent and Triton X-114, equilibrating temperature and centrifuging time were evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. The preconcentration factor was found to be (50-fold) for 250 ml of water sample. Under optimum condition the detection limit was found as 0.067 ngml(-1) for palladium in various environmental matrices. The present method was applied for the determination of palladium in various water samples, alloys and the result shows good agreement with reported method and the recoveries are in the range of 96.7-99.4%.

Novel analytical reagent for the application of cloud-point preconcentration and flame atomic absorption spectrometric determination of nickel in natural water samples.

Cloud-point extraction was applied as a preconcentration of nickel after formation of complex with newly synthesized N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine, and later determined by flame atomic absorption spectrometry (FAAS) using octyl phenoxy polyethoxy ethanol (Triton X-114) as surfactant. Nickel was complexed with N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine in an aqueous phase and was kept for 15 min in a thermo-stated bath at 40 degrees C. Separation of the two phases was accomplished by centrifugation for 15 min at 4000 rpm. The chemical variables affecting the cloud-point extraction were evaluated, optimized and successfully applied to the nickel determination in various water samples. Under the optimized conditions, the preconcentration system of 100 ml sample permitted an enhancement factor of 50-fold. The detailed study of various interferences made the method more selective. The detection limits obtained under optimal condition was 0.042 ngml(-1). The extraction efficiency was investigated at different nickel concentrations (20-80 ngml(-1)) and good recoveries (99.05-99.93%) were obtained using present method. The proposed method has been applied successfully for the determination of nickel in various water samples and compared with reported method in terms of Student's t-test and variance ratio f-test which indicate the significance of present method over reported and spectrophotometric methods at 95% confidence level.

Facile and sensitive spectrophotometric determination of synthetic pyrithroids in their formulations, water and grain samples.

A novel reagent was introduced for the facile and sensitive spectrophotometric determination of synthetic pyrethroids in their formulations (fenvalerate, cypermethrin and decamethrin), water and grain samples. These methods were based on the hydrolysis of synthetic pyrethroids under the alkaline conditions to form respective aldehyde groups. These groups were condensation with 3-methyl-2-benzothiazolinone hydrochloride (MBTH) to yield color derivatives having lambda(max) at 520 nm for fenvalerate, 516 nm for cypermethrin and 512 nm for decamethrin. The proposed method could be successfully applied for the determination of synthetic pyrethroids in their formulations, water and grain samples.

RETRACTED: Preconcentration and solid-phase extraction of beryllium, lead, nickel, and bismuth from various water samples using 2-propylpiperidine-1-carbodithioate with flame atomic absorption spectrometry (FAAS).

This article has been retracted at the request of the Editors-in-Chief. Please see Elsevier Policy on Article Withdrawal (http://www.elsevier.com/locate/withdrawalpolicy). REASON: Considerable concern was raised about the research purportedly conducted at Sri Venkateswara University, India with the alleged involvement of Professor P. Chiranjeevi. Questions were raised as to the volume of publications, the actual capacity (equipment, orientation and chemicals) of the laboratory in which Professor Chiranjeevi worked, the validity of certain of the research data identified in the articles, the fact that a number of papers appear to have been plagiarized from other previously published papers, and some aspects of authorship. Professor Chiranjeevi was given the opportunity to respond to these allegations. Thereafter, a committee was constituted by the University to look into these allegations. Based on the enquiry committee report, we have been informed by the head of the Department of Chemistry at Sri Venkateswara University that the university authorities have taken disciplinary action against Professor Chiranjeevi, as the university considers that there are grounds for such action. Therefore, based on the results of this investigation, the Editors-in-Chief are retracting this article.

Studies of selenium in environmental samples and synthetic mixtures by spectrophotometry.

A rapid, highly sensitive and selective spectrophotometric method for the determination of traces of selenium(IV) is described. The method is based on oxidation of p-nitroaniline by selenium(IV) followed by coupling reaction with N-(1-naphthalene-1-yl)ethane-1,2-diamine dihydrochloride (NEDA) in neutral medium to give red colored derivative with lambda(max) 515 nm and is stable for more than 10 days at 35 degrees C. Beer's law is obeyed for selenium(IV) in the concentration range of 0.02-3.2 microg ml(-1) at the wavelength of maximum absorption. The optimum reaction conditions and other analytical parameters were investigated to enhance the sensitivity of the present method. The detailed study of various interferences made the method more selective. The proposed method was successfully applied to the analysis of selenium in polluted water, natural water samples, plant material, soil samples, and synthetic mixtures. The results obtained were agreed with the reported methods at the 95% confidence level. The performance of proposed method was evaluated in terms of Student's t-test and Variance ratio f-test which indicates the significance of proposed method over reported method.

Extractive spectrofluorometric determination of quinalphos using fluorescein in environmental samples.

A simple, sensitive, convenient and low cost spectrofluorometric technique for determination of quinalphos is described. Quinalphos is decomposed with sodium ethoxide. Resultant sodium diethyl thiophosphate (Na-DETP) is extracted with a cationic fluorescein as ion pair complex into 1-chloro-2-nitrobenzene. The fluorescence of the ion pair, fluorescein-DETP is measured at 530 nm after excitation at 490 nm. This technique is applicable for the determination of quinalphos in water, food grains and vegetable samples up to ng level with Amberlite XAD-4.

The facile flow-injection spectrophotometric detection of gold(III) in water and pharmaceutical samples using 3,5-dimethoxy-4-hydroxy-2-aminoacetophenone isonicotinoyl hydrazone (3,5-DMHAAINH).

A simple, sensitive and rapid flow-injection spectrophotometric method was developed for the determination of trace amounts of Au(III) in aqueous dimethylformamide (DMF). The method is based on formation of Au(III)-(3,5-DMHAAINH)3 complex. The optimum conditions for the chromogenic reaction of Au(III) with 3,5-DMHAAINH is studied and the colored (reddish brown) complex is selectively monitored at lambda(max) 490 nm at pH 6.0. The reaction and flow conditions of the full experimental design were optimized. The detection limit (2 s) of 0.1 microg l-1 Au(III) was obtained at a sampling rate of 15 samples h-1. Beer's law is obeyed over the range of 0.30-4.00 microg ml-1. The molar absorptivity and Sandell's sensitivity were 3.450x10(4) M and 0.0050 microg ml-1, respectively. Job's method of continuous variation and stability constants corresponding to these maxima was determined and found to be 9.3x10(15) (1:3, M:R) (M, metal; R, reagent). The detailed study of various interferences confirmed the high selectivity of the developed method. The method was successfully applied for the determination of trace amount of Au(III) in water and pharmaceutical samples. The results obtained were in agreement with the reported methods at the 95% confidence level.

RETRACTED: Simultaneous flow-through determination of nitrites, nitrates and their mixtures in environmental and biological samples using spectrophotometry.

This article has been retracted at the request of the Editors-in-Chief. Please see Elsevier Policy on Article Withdrawal (http://www.elsevier.com/locate/withdrawalpolicy). REASON: Considerable concern was raised about the research purportedly conducted at Sri Venkateswara University, India with the alleged involvement of Professor P. Chiranjeevi. Questions were raised as to the volume of publications, the actual capacity (equipment, orientation and chemicals) of the laboratory in which Professor Chiranjeevi worked, the validity of certain of the research data identified in the articles, the fact that a number of papers appear to have been plagiarized from other previously published papers, and some aspects of authorship. Professor Chiranjeevi was given the opportunity to respond to these allegations. Thereafter, a committee was constituted by the University to look into these allegations. Based on the enquiry committee report, we have been informed by the head of the Department of Chemistry at Sri Venkateswara University that the university authorities have taken disciplinary action against Professor Chiranjeevi, as the university considers that there are grounds for such action. Therefore, based on the results of this investigation, the Editors-in-Chief are retracting this article.

The determination of nickel(II) after on-line sorbent preconcentration by inductively coupled plasma atomic emission spectrometry using Borassus Flabellifer inflorescence loaded with coniine dithiocarbamate.

A procedure was developed for the determination of nickel(II) in water samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) after preconcentration on coniine dithiocarbamate (CDC) supported by Borassus Flabellifer inflorescence. The sorbed element was subsequently eluted with 0.4M nitric acid and the acid eluates are analysed by ICP-AES. The influence of various parameters such as pH, flow rate of sample, eluent concentration, volume of the sample and volume eluent were investigated. Under the optimal conditions, nickel in aqueous sample was concentrated about 100-fold. Nickel recovery was obtained by the proposed method in range of 98.9-99.9%. This method is also applied for the analysis of spiked and natural water samples. The results provide strong evidence to support the hypothesis of an adsorption mechanism.