New Analytical Technique For The Determination Of Mercury (II) By Synergistic Extractive Spectrophotometric Method With N'',N'''-Bis[(E)-(4-fluorophenyl)methylidene] Thiocarbonohydrazide
A new technique was developed for the extractive spectrophotometric determination of mercury (II) by using newly synthesized chromogenic reagent N'',N'''-bis[(E)-(4-fluorophenyl)methylidene] thiocarbonohydrazide bis-(4-fluoroPM)TCH. It forms yellow colored ternary complex with mercury(II) in presence pyridine having composition 1:1:1 (M:Reagent:Py) in acidic pH range 1.7-3.7. The reagent is highly sensitive and selective towards mercury(II). So spectrophotometric method of mercury(II) is found to be very rapid, reliable and show synergistic effect. Absorption of colored organic layer in iso amyl acetate is measured with reagent blank at λmax 375 nm. Pyridine showed synergistic effect with reagent by the adduct formation in organic phase. Beer’s law was obeyed in the concentration range 0.25 to 3.5 µg mL-1 for mercury (II). Molar absorptivity and sandell’s sensitivity values of mercury(II)-bis-(4-fluoroPM)TCH-Py complex are 0.50127x105 lit mol-1 cm -1 and 0.004 µg cm -2 , respectively. The selectivity of the method was checked by using various foreign ions. The composition of the complex was determined by slope ratio method, mole ratio method and Job’s method of continuous variation. The colour of ternary complex was stable for more than 12 h. Various factors influencing on degree of comlexation are the effect of pH, reagent concentration, synergent concentration, equilibrium time, solvent were determined. The method was applicable for determination of mercury(II) in binary mixture, ternary mixture, ayurvedic sample, homoeopathic sample, industrial waste water, spiked water and dental unit waste water.
Engineering Research Publication
Best International Journals, High Impact Journals,
International Journal of Engineering & Technical Research
ISSN : 2321-0869 (O) 2454-4698 (P)
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SYNTHESIS AND CHARACTERIZATION OF KAOLINITE COATED WITH CU-OXIDE AND ITS EFFE...Premier Publishers
In this paper, a novel copper oxide coated kaolinite was prepared as an adsorbent of Hg(II) ions from aqueous media. The materials used for this study were synthesized, characterised and the product tested for mercury ion removal using standard laboratory procedures. Reactivity and removal kinetic models derived from Freundlich isotherm were used to investigate contact time and pH effects on the coefficient of protonation and rate of mass transfer of Hg(II) ions to the reactive sites, Proton coefficient of 0.89 indicated a decrease in proton consumption function when compared with uncoated kaolinite. At the 12th h reaction time, a maximum adsorption capacity of 85% was achieved. Mass transfer rates of 0.9359h-1 and 0.0748h-1 for the first and second reaction phases indicated a reduction when compared with uncoated kaolinite. These changes may be ascribed to masking of reaction sites and exposed surface area of the Cu-Oxide coated kaolinite.
IJERA (International journal of Engineering Research and Applications) is International online, ... peer reviewed journal. For more detail or submit your article, please visit www.ijera.com
IOSR Journal of Applied Chemistry (IOSR-JAC) is an open access international journal that provides rapid publication (within a month) of articles in all areas of applied chemistry and its applications. The journal welcomes publications of high quality papers on theoretical developments and practical applications in Chemical Science. Original research papers, state-of-the-art reviews, and high quality technical notes are invited for publications.
Engineering Research Publication
Best International Journals, High Impact Journals,
International Journal of Engineering & Technical Research
ISSN : 2321-0869 (O) 2454-4698 (P)
www.erpublication.org
SYNTHESIS AND CHARACTERIZATION OF KAOLINITE COATED WITH CU-OXIDE AND ITS EFFE...Premier Publishers
In this paper, a novel copper oxide coated kaolinite was prepared as an adsorbent of Hg(II) ions from aqueous media. The materials used for this study were synthesized, characterised and the product tested for mercury ion removal using standard laboratory procedures. Reactivity and removal kinetic models derived from Freundlich isotherm were used to investigate contact time and pH effects on the coefficient of protonation and rate of mass transfer of Hg(II) ions to the reactive sites, Proton coefficient of 0.89 indicated a decrease in proton consumption function when compared with uncoated kaolinite. At the 12th h reaction time, a maximum adsorption capacity of 85% was achieved. Mass transfer rates of 0.9359h-1 and 0.0748h-1 for the first and second reaction phases indicated a reduction when compared with uncoated kaolinite. These changes may be ascribed to masking of reaction sites and exposed surface area of the Cu-Oxide coated kaolinite.
IJERA (International journal of Engineering Research and Applications) is International online, ... peer reviewed journal. For more detail or submit your article, please visit www.ijera.com
IOSR Journal of Applied Chemistry (IOSR-JAC) is an open access international journal that provides rapid publication (within a month) of articles in all areas of applied chemistry and its applications. The journal welcomes publications of high quality papers on theoretical developments and practical applications in Chemical Science. Original research papers, state-of-the-art reviews, and high quality technical notes are invited for publications.
Equilibrium and Kinetics Adsorption of Cadmium and Lead Ions from Aqueous Sol...theijes
Sourcing cheap adsorbents for the treatment of waste water is imperative for local environments. The adsorption of cadmium (Cd) and lead (Pb) from aqueous solution onto bamboo activated carbon prepared by chemical activation with ZnCl2 was investigated. The unwashed chemical activated bamboo carbon (UCABC) achieved up to 87.81% and 96.45% removal of Cd and Pb at pH-5 and 11, respectively. Removal equilibrium was attained within 1hr and 2.5hrs for Cd and Pb, respectively. The Cd and Pb adsorption increased with adsorbent dosage decrease while removal rate (%) increased with Cd and Pb concentration. Adsorption isotherm of Cd and Pb onto UCABC was determined and correlated with four isotherm models (Langmuir, Freundlich, Temkin and Hills). The equilibrium data fitted into Freundlich Cd (R2 = 0.9873, SSE = 0.045), Pb (R2 =0.9903, SSE = 0.051); Temkin Cd (R2 =0.9730, SSE = 0.052), Pb (R2 = 0.9079, SSE = 0.056); Hills Cd (R2 = 0.9961, SSE = 0.048), Pb (R2.= 0.9183, SSE = 0.053) and Langmuir Cd (R2 = 0.9653, SSE = 0.302), Pb (R2 = 0.9899, SSE = 0.136) isotherms. The Freundlich fitting showed isotherm adsorption capacity constants Kf = 7.843 and 5.098 (mg/g) for Cd and Pb, respectively. Furthermore, their adsorption kinetics correlated with the Pseudo-first order, Pseudo-second order and Intra-particle diffusion models and could be best described by the Pseudo-second order equation, suggesting chemisorptions as the limiting process. This study demonstrated that the UCABC can remove Cd2+ and Pb+ ions from aqueous solution to avert expensive commercial adsorbents
Removal of Cu(II) Ions from Aqueous Solutions by Adsorption Onto Activated Ca...IJERA Editor
This paper studied the ability of using local activated carbon (LAC) derived from olive waste cakes as an
adsorbent for the removal of Cu(II) ions from aqueous solution by batch operation. Various operating parameters
such as solution pH, adsorbent dosage, initial metal ions concentration, and equilibrium contact time have been
studied. The results indicated that the adsorption of Cu(II) increased with the increasing pH, and the optimum
solution pH for the adsorption of Cu(II) was found to be 5. The adsorption process increases with increasing
dosage of LAC, also the amount of Cu(II) removed changes with Cu(II) initial concentration and contact time.
Adsorption was rapid and occurred within 25 min. for Cu(II) concentration range from 60 to 120 mg/l
isothermally at 30±1 oC. Maximum adsorption occurs at Cu(II) initial concentration lesser than 100 mg/l by
using adsorbent dosage (1.2 g/l). The equilibrium adsorption data for Cu(II) were fitted well with the Langmuir
and Freundlich adsorption isotherm models. The maximum adsorption capacity of LAC was found to be 106.383
mg/g. So, the results indicated the suitability use of the activated carbon derived from olive waste cakes (LAC)
as low cost and natural material for reliable removal of Cu(II) from water and wastewater effluents.
Solvent Extraction Method for the Separation of Cerium(III) as
Cations From Aqueous Media By use 4-[N-(5-methyl isoxazol-3-
yl)benzene sulfonamide azo]-1- Naphthol Coupled With
Spectroscopic Method For Determination
A new Schiff base 4-chlorophenyl)methanimine
(6R,7R)-3-methyl-8-oxo-7-(2-phenylpropanamido)-5-thia-1-
azabicyclo[4.2.0]oct-2-ene-2-carboxylate= (HL)= C23H20
ClN3O4S) has been synthesized from β-lactam antibiotic
(cephalexin mono hydrate(CephH)=(C16H19N3O5S.H2O) and 4-
chlorobenzaldehyde . Figure(1) Metal mixed ligand complexes
of the Schiff base were prepared from chloride salt of
Fe(II),Co(II),Ni(II),Cu(II),Zn(II) and Cd (II), in 50% (v/v)
ethanol –water medium (SacH ) .in aqueous ethanol(1:1)
containing and Saccharin(C7H5NO3S) = sodium hydroxide.
Several physical tools in particular; IR, CHN, 1H NMR, 13C
NMR for ligand and melting point molar conductance, magnetic
moment. and determination the percentage of the metal in the
complexes by flame(AAS). The ligands and there metal
complexes were screened for their antimicrobial activity against
four bacteria (gram + ve) and (gram -ve) {Escherichia coli,
Pseudomonas aeruginosa, Staphylococcus aureus and Bacillus}.
The proposed structure of the complexes using program, Chem
office 3D(2006). The general formula have been given for the
prepared mixed ligand complexes Na2[M(Sac)3(L)], M(II) = Fe
(II), Co(II) , Ni(II), Cu (II), Zn(II) , and Cd(II).
HL= C29H24 ClN3O4S, L= C29H23 ClN3O4S -.
Isotherm Modeling and Thermodynamic Study of the Adsorption of Toxic Metal by...CrimsonpublishersEAES
Isotherm Modeling and Thermodynamic Study of the Adsorption of Toxic Metal by the Apricot Stone by Moussa Abbas*, Tounsia Aksil and Mohamed Trari in Environmental Analysis & Ecology Studies
Using Tunisian Phosphate Rock and Her Converted Hydroxyapatite for Lead Remov...IJERA Editor
Natural and synthesis apatites represent a cost effective soil amendment, which can be used for in situ reduction of lead bioavailability and mobility. In our previous work, we selected Tunisian Phosphate Rock (TPR) and Hydroxyapatite (CaHAp) as promising minerals for the removal of lead from aqueous solutions. X-ray powder diffraction patterns (DRX), Infra Red (IR), Thermogravimetric analysis (TGA) and Scanning Electron Microscopy (SEM) were used to characterize TPR and CaHAp. CaHAp was prepared from TPR and employed for the removal of Pb2+ ions at different concentrations from aqueous solution to determine the adsorption properties of CaHAp and compare them with those of a TPR. The kinetic data obtained indicated that the adsorption performances of the adsorbents depended both on their specific surface area and crystallinity. Complexation of lead ion on the adsorbent surface favoured the dissolution of hydroxyapatites characterized by a Ca/Pb molar ratio of 1.69. The maximum adsorption capacity of CaHAp for Pb2+ ions at 25 °C was 1.806 mmol /g relative to 1.035 mmol /g for TPR at the same temperature. The higher capacity of CaHAp was explained in terms of its porosity and crystallinity. The Pb2+ ions sorption results could be modelled by the Langmuir and Freundlich isotherms. The simulations of adsorption isotherms of Pb2+ on CaHAp allow us to conclude that there is a good correlation between the experimental data and the Langmuir model. On TPR, we show a good correlation between the experimental data and the Langmuir and Freundlich model.
Eco-friendly method for the estimation of cobalt (II) in real samples using 1...Innspub Net
An easy and quick spectrophotometric method is developed for the investigation of cobalt at trace level using 1-(2-Thiazolylazo)-2-naphthol (TAN) in presence of surfactant cetyltrimethylammonium bromide (CTAB) aqueous micellar solution. The cobalt forms bis [1-(2-Thiazolylazo)-2-naphthol] cobalt complex reacting with 1-(2-Thiazolylazo)-2-naphthol. Proposed method is of great importance because use of micellar system instead of solvent extraction steps that were toxic, expensive and time consuming. The method shows improved sensitivity, selectivity and molar absorption. The coefficient of molar absorption and Sandell’s sensitivity was found to be ε 1.89 × 104L mol-1 cm-1 and 3.1ngcm-2 at λmax 572.7nm. Graph of Linear concentration calibration was obtained in the range 0.02-9.0μgmL-1; stoichiometric metal ligand ratio was found 1:2 for the complex Co-[TAN]2 formation. The proposed method was applied for the investigation of cobalt from different alloys, biological, environmental and pharmaceutical samples. Full articles at https://lnkd.in/fbEHTJ6
Examination of Adsorption Abilities of Natural and Acid Activated Bentonite f...AnuragSingh1049
The effect of the initial concentration of Cr, Co, Cu, Ni, and Pb metal ions from multicomponent solutions on the sorption capacity of natural and acid activated bentonite was examined in this paper. The acid activation was performed by using hydrochloric and sulfuric acid at different concentrations. The results of adsorption research have shown that bentonite can be effectively used as an adsorbent for the removal of metal ions from multicomponent solutions. Acid activation of bentonite changes the structure and content of individual oxides, increases the porosity and the number of available spots for the adsorption process. For this reason, the bentonite removal efficiency increased after acid activation for all heavy metals tested. With increased acid concentration, the degree of bentonite adsorption increased, and sulfuric acid rather than chloric acid showed better results in removal efficiency.
Photocatalytic Degradation of Ciprofloxacin using TiO2 in a Slurry Photocatal...ijtsrd
A slurry photocatalytic reactor assessed for the degradation of ciprofloxacin CFX . The effect of operating parameters like initial ciprofloxacin concentration, catalyst dosage and pH on ciprofloxacin degradation was analysed in this study. Batch study was conducted and it showed 90 degradation of the CFX. It was observed the optimum concentration of CFX was 1500 µg l, catalyst dosage was 1 g l at the pH of 9 for the duration of 3 hours. The photocatalytic degradation of CFX followed the pseudo first order kinetics. Karthika. V | Vedavalli. S | Afreen Begum. M "Photocatalytic Degradation of Ciprofloxacin using TiO2 in a Slurry Photocatalytic Reactor: Optimization" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-4 | Issue-4 , June 2020, URL: https://www.ijtsrd.com/papers/ijtsrd31224.pdf Paper Url :https://www.ijtsrd.com/engineering/environment-engineering/31224/photocatalytic-degradation-of-ciprofloxacin-using-tio2-in-a-slurry-photocatalytic-reactor-optimization/karthika-v
This study aims to employ low-cost agro waste
biosorbent tamarind (Tamarindus indica) pod shells and
activated carbon prepared by complete and partial pyrolysis of
tamarind pod shell for the removal of hexavalent chromium
ions from aqueous solution. The effect of parameters namely,
initial metal ion concentration, pH, temperature, biomass
loading on chromium removal efficiency were studied. More
than 96.9% removal of Chromium was achieved using crude
tamarind pod shells as biosorbent. The experimental data
obtained were fitted with Langmuir, Freundlich, Temkin and
Redlich-Peterson adsorption isotherm models. The
experimental data fits well to Langmuir, Freundlich and
Temkin isotherms with regression coefficient R2 more than 0.9.
For Redlich-Peterson adsorption isotherm the experimental
data does not fit so well. The crude tamarind had maximum
monolayer adsorption capacity of 40 mg/g and a separation
factor of 0.0416 indicating it as best adsorbent among the three
tested adsorbent. Further, an attempt is made to fit sorption
kinetics with pseudo first order and pseudo second order
reactions. Pseudo second order kinetics model fits well to the
experimental data for all three adsorbents.
Removal of chromium (vi) by activated carbon derived from mangifera indicaeSAT Publishing House
IJRET : International Journal of Research in Engineering and Technology is an international peer reviewed, online journal published by eSAT Publishing House for the enhancement of research in various disciplines of Engineering and Technology. The aim and scope of the journal is to provide an academic medium and an important reference for the advancement and dissemination of research results that support high-level learning, teaching and research in the fields of Engineering and Technology. We bring together Scientists, Academician, Field Engineers, Scholars and Students of related fields of Engineering and Technology
Potato peels which are a low cost, renewable agroindustry by-product were used for the removal of hexavalent chromium from
aqueous effluents. Batch experiments were carried out with an artificial effluent comprising of potassium dichromate in deionised
water. The effects of the initial hexavalent chromium concentration, dose of biosorbent, and removal kinetics were explored. An
adsorbent dosage of 4 g/L was effective in complete removal of the metal ion, at pH 2.5, in 48 minutes. The kinetic process of
Cr(VI) adsorption onto potato peel powder was tested by applying pseudo-first-order and pseudo-second-order models as well as
the Elovich kinetic equation to correlate the experimental data and to determine the kinetic parameters. The adsorption data were
correlated by the Langmuir and Freundlich isotherms. A maximum monolayer adsorption capacity of 3.28 mg/g was calculated
using the Langmuir adsorption isotherm, suggesting a functional group limited adsorption process. The results confirmed that
potato peels are an effective biosorbent for the removal of hexavalent chromium from effluent.
Adsorption Studies of an Acid Dye From Aqueous Solution Using Lagerstroemia ...IJMER
The effectiveness of adsorption for acid dye removal from wastewaters has made it an ideal alternative to other expensive treatment options. The removal of acid Violet 4BS onto seeds of Lagerstroemia indica (LIS) from aqueous solutions was investigated using parameters such as contact time, pH, temperature, adsorbent doses, and initial dye concentration. Adsorption isotherms of dyes onto LIS were determined and correlated with common isotherm equations such as the Langmuir and
Freundlich models. It was found that the Langmuir isotherm appears to fit the isotherm data better than
the Freundlich isotherm. Parameters of the Langmuir and Freundlich isotherms were determined using adsorption data. The maximum removal of Acid Violet 4BS by the adsorbent was obtained at pH 2. The maximum percentage of dye removal (86.67%) was obtained at an initial dye concentration of 10mg/L with adsorbent dosage of 50 mg per 50 ml of dye solution. The adsorption kinetics of acid violet 4BS could be described by the pseudo-second order reaction model. The data obtained from adsorption
isotherms at different temperatures were used to calculate several thermo-dynamic quantities such as the
Gibbs energy (ΔG0), enthalpy (ΔH0), and entropy (ΔS
0) of adsorption. The adsorption process was found
to be spontaneous, exothermic and physical in nature. Locally available adsorbent LIS was found to have
a low cost and was promising for the removal of acid violet 4BS from aqueous solutions
While document and file sharing is increasing rapidly, 97% of organizations cite file sharing as a high risk for information loss, and 75% believe their organization is currently at risk for data loss.
A SEMI-BLIND WATERMARKING SCHEME FOR RGB IMAGE USING CURVELET TRANSFORMijfcstjournal
In this paper, a semi-blind watermarking technique of embedding the color watermark using curvelet
coefficient in RGB cover image has been proposed. The technique used the concept of HVS that the human
eyes are not much sensitive to blue color. So the blue color plane of the cover image is used as embedding
domain. A bit planes method is also used, the most significant bit (MSB) plane of watermark image is used
as embedding information. Selected scale and orientation of the curvelet coefficients of the blue channel in
the cover image has been used for embedding the watermark information. All other 0-7 bit planes are used
as a key at the time of extraction. The results of the watermarking scheme have been analyzed by different
quality assessment metric such as PSNR, Correlation Coefficient (CC) and Mean Structure Similarity Index
Measure (MSSIM). The experimental results show that the proposed technique gives the good invisibility of
watermark, quality of extracted watermark and robustness against different attacks.
Equilibrium and Kinetics Adsorption of Cadmium and Lead Ions from Aqueous Sol...theijes
Sourcing cheap adsorbents for the treatment of waste water is imperative for local environments. The adsorption of cadmium (Cd) and lead (Pb) from aqueous solution onto bamboo activated carbon prepared by chemical activation with ZnCl2 was investigated. The unwashed chemical activated bamboo carbon (UCABC) achieved up to 87.81% and 96.45% removal of Cd and Pb at pH-5 and 11, respectively. Removal equilibrium was attained within 1hr and 2.5hrs for Cd and Pb, respectively. The Cd and Pb adsorption increased with adsorbent dosage decrease while removal rate (%) increased with Cd and Pb concentration. Adsorption isotherm of Cd and Pb onto UCABC was determined and correlated with four isotherm models (Langmuir, Freundlich, Temkin and Hills). The equilibrium data fitted into Freundlich Cd (R2 = 0.9873, SSE = 0.045), Pb (R2 =0.9903, SSE = 0.051); Temkin Cd (R2 =0.9730, SSE = 0.052), Pb (R2 = 0.9079, SSE = 0.056); Hills Cd (R2 = 0.9961, SSE = 0.048), Pb (R2.= 0.9183, SSE = 0.053) and Langmuir Cd (R2 = 0.9653, SSE = 0.302), Pb (R2 = 0.9899, SSE = 0.136) isotherms. The Freundlich fitting showed isotherm adsorption capacity constants Kf = 7.843 and 5.098 (mg/g) for Cd and Pb, respectively. Furthermore, their adsorption kinetics correlated with the Pseudo-first order, Pseudo-second order and Intra-particle diffusion models and could be best described by the Pseudo-second order equation, suggesting chemisorptions as the limiting process. This study demonstrated that the UCABC can remove Cd2+ and Pb+ ions from aqueous solution to avert expensive commercial adsorbents
Removal of Cu(II) Ions from Aqueous Solutions by Adsorption Onto Activated Ca...IJERA Editor
This paper studied the ability of using local activated carbon (LAC) derived from olive waste cakes as an
adsorbent for the removal of Cu(II) ions from aqueous solution by batch operation. Various operating parameters
such as solution pH, adsorbent dosage, initial metal ions concentration, and equilibrium contact time have been
studied. The results indicated that the adsorption of Cu(II) increased with the increasing pH, and the optimum
solution pH for the adsorption of Cu(II) was found to be 5. The adsorption process increases with increasing
dosage of LAC, also the amount of Cu(II) removed changes with Cu(II) initial concentration and contact time.
Adsorption was rapid and occurred within 25 min. for Cu(II) concentration range from 60 to 120 mg/l
isothermally at 30±1 oC. Maximum adsorption occurs at Cu(II) initial concentration lesser than 100 mg/l by
using adsorbent dosage (1.2 g/l). The equilibrium adsorption data for Cu(II) were fitted well with the Langmuir
and Freundlich adsorption isotherm models. The maximum adsorption capacity of LAC was found to be 106.383
mg/g. So, the results indicated the suitability use of the activated carbon derived from olive waste cakes (LAC)
as low cost and natural material for reliable removal of Cu(II) from water and wastewater effluents.
Solvent Extraction Method for the Separation of Cerium(III) as
Cations From Aqueous Media By use 4-[N-(5-methyl isoxazol-3-
yl)benzene sulfonamide azo]-1- Naphthol Coupled With
Spectroscopic Method For Determination
A new Schiff base 4-chlorophenyl)methanimine
(6R,7R)-3-methyl-8-oxo-7-(2-phenylpropanamido)-5-thia-1-
azabicyclo[4.2.0]oct-2-ene-2-carboxylate= (HL)= C23H20
ClN3O4S) has been synthesized from β-lactam antibiotic
(cephalexin mono hydrate(CephH)=(C16H19N3O5S.H2O) and 4-
chlorobenzaldehyde . Figure(1) Metal mixed ligand complexes
of the Schiff base were prepared from chloride salt of
Fe(II),Co(II),Ni(II),Cu(II),Zn(II) and Cd (II), in 50% (v/v)
ethanol –water medium (SacH ) .in aqueous ethanol(1:1)
containing and Saccharin(C7H5NO3S) = sodium hydroxide.
Several physical tools in particular; IR, CHN, 1H NMR, 13C
NMR for ligand and melting point molar conductance, magnetic
moment. and determination the percentage of the metal in the
complexes by flame(AAS). The ligands and there metal
complexes were screened for their antimicrobial activity against
four bacteria (gram + ve) and (gram -ve) {Escherichia coli,
Pseudomonas aeruginosa, Staphylococcus aureus and Bacillus}.
The proposed structure of the complexes using program, Chem
office 3D(2006). The general formula have been given for the
prepared mixed ligand complexes Na2[M(Sac)3(L)], M(II) = Fe
(II), Co(II) , Ni(II), Cu (II), Zn(II) , and Cd(II).
HL= C29H24 ClN3O4S, L= C29H23 ClN3O4S -.
Isotherm Modeling and Thermodynamic Study of the Adsorption of Toxic Metal by...CrimsonpublishersEAES
Isotherm Modeling and Thermodynamic Study of the Adsorption of Toxic Metal by the Apricot Stone by Moussa Abbas*, Tounsia Aksil and Mohamed Trari in Environmental Analysis & Ecology Studies
Using Tunisian Phosphate Rock and Her Converted Hydroxyapatite for Lead Remov...IJERA Editor
Natural and synthesis apatites represent a cost effective soil amendment, which can be used for in situ reduction of lead bioavailability and mobility. In our previous work, we selected Tunisian Phosphate Rock (TPR) and Hydroxyapatite (CaHAp) as promising minerals for the removal of lead from aqueous solutions. X-ray powder diffraction patterns (DRX), Infra Red (IR), Thermogravimetric analysis (TGA) and Scanning Electron Microscopy (SEM) were used to characterize TPR and CaHAp. CaHAp was prepared from TPR and employed for the removal of Pb2+ ions at different concentrations from aqueous solution to determine the adsorption properties of CaHAp and compare them with those of a TPR. The kinetic data obtained indicated that the adsorption performances of the adsorbents depended both on their specific surface area and crystallinity. Complexation of lead ion on the adsorbent surface favoured the dissolution of hydroxyapatites characterized by a Ca/Pb molar ratio of 1.69. The maximum adsorption capacity of CaHAp for Pb2+ ions at 25 °C was 1.806 mmol /g relative to 1.035 mmol /g for TPR at the same temperature. The higher capacity of CaHAp was explained in terms of its porosity and crystallinity. The Pb2+ ions sorption results could be modelled by the Langmuir and Freundlich isotherms. The simulations of adsorption isotherms of Pb2+ on CaHAp allow us to conclude that there is a good correlation between the experimental data and the Langmuir model. On TPR, we show a good correlation between the experimental data and the Langmuir and Freundlich model.
Eco-friendly method for the estimation of cobalt (II) in real samples using 1...Innspub Net
An easy and quick spectrophotometric method is developed for the investigation of cobalt at trace level using 1-(2-Thiazolylazo)-2-naphthol (TAN) in presence of surfactant cetyltrimethylammonium bromide (CTAB) aqueous micellar solution. The cobalt forms bis [1-(2-Thiazolylazo)-2-naphthol] cobalt complex reacting with 1-(2-Thiazolylazo)-2-naphthol. Proposed method is of great importance because use of micellar system instead of solvent extraction steps that were toxic, expensive and time consuming. The method shows improved sensitivity, selectivity and molar absorption. The coefficient of molar absorption and Sandell’s sensitivity was found to be ε 1.89 × 104L mol-1 cm-1 and 3.1ngcm-2 at λmax 572.7nm. Graph of Linear concentration calibration was obtained in the range 0.02-9.0μgmL-1; stoichiometric metal ligand ratio was found 1:2 for the complex Co-[TAN]2 formation. The proposed method was applied for the investigation of cobalt from different alloys, biological, environmental and pharmaceutical samples. Full articles at https://lnkd.in/fbEHTJ6
Examination of Adsorption Abilities of Natural and Acid Activated Bentonite f...AnuragSingh1049
The effect of the initial concentration of Cr, Co, Cu, Ni, and Pb metal ions from multicomponent solutions on the sorption capacity of natural and acid activated bentonite was examined in this paper. The acid activation was performed by using hydrochloric and sulfuric acid at different concentrations. The results of adsorption research have shown that bentonite can be effectively used as an adsorbent for the removal of metal ions from multicomponent solutions. Acid activation of bentonite changes the structure and content of individual oxides, increases the porosity and the number of available spots for the adsorption process. For this reason, the bentonite removal efficiency increased after acid activation for all heavy metals tested. With increased acid concentration, the degree of bentonite adsorption increased, and sulfuric acid rather than chloric acid showed better results in removal efficiency.
Photocatalytic Degradation of Ciprofloxacin using TiO2 in a Slurry Photocatal...ijtsrd
A slurry photocatalytic reactor assessed for the degradation of ciprofloxacin CFX . The effect of operating parameters like initial ciprofloxacin concentration, catalyst dosage and pH on ciprofloxacin degradation was analysed in this study. Batch study was conducted and it showed 90 degradation of the CFX. It was observed the optimum concentration of CFX was 1500 µg l, catalyst dosage was 1 g l at the pH of 9 for the duration of 3 hours. The photocatalytic degradation of CFX followed the pseudo first order kinetics. Karthika. V | Vedavalli. S | Afreen Begum. M "Photocatalytic Degradation of Ciprofloxacin using TiO2 in a Slurry Photocatalytic Reactor: Optimization" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-4 | Issue-4 , June 2020, URL: https://www.ijtsrd.com/papers/ijtsrd31224.pdf Paper Url :https://www.ijtsrd.com/engineering/environment-engineering/31224/photocatalytic-degradation-of-ciprofloxacin-using-tio2-in-a-slurry-photocatalytic-reactor-optimization/karthika-v
This study aims to employ low-cost agro waste
biosorbent tamarind (Tamarindus indica) pod shells and
activated carbon prepared by complete and partial pyrolysis of
tamarind pod shell for the removal of hexavalent chromium
ions from aqueous solution. The effect of parameters namely,
initial metal ion concentration, pH, temperature, biomass
loading on chromium removal efficiency were studied. More
than 96.9% removal of Chromium was achieved using crude
tamarind pod shells as biosorbent. The experimental data
obtained were fitted with Langmuir, Freundlich, Temkin and
Redlich-Peterson adsorption isotherm models. The
experimental data fits well to Langmuir, Freundlich and
Temkin isotherms with regression coefficient R2 more than 0.9.
For Redlich-Peterson adsorption isotherm the experimental
data does not fit so well. The crude tamarind had maximum
monolayer adsorption capacity of 40 mg/g and a separation
factor of 0.0416 indicating it as best adsorbent among the three
tested adsorbent. Further, an attempt is made to fit sorption
kinetics with pseudo first order and pseudo second order
reactions. Pseudo second order kinetics model fits well to the
experimental data for all three adsorbents.
Removal of chromium (vi) by activated carbon derived from mangifera indicaeSAT Publishing House
IJRET : International Journal of Research in Engineering and Technology is an international peer reviewed, online journal published by eSAT Publishing House for the enhancement of research in various disciplines of Engineering and Technology. The aim and scope of the journal is to provide an academic medium and an important reference for the advancement and dissemination of research results that support high-level learning, teaching and research in the fields of Engineering and Technology. We bring together Scientists, Academician, Field Engineers, Scholars and Students of related fields of Engineering and Technology
Potato peels which are a low cost, renewable agroindustry by-product were used for the removal of hexavalent chromium from
aqueous effluents. Batch experiments were carried out with an artificial effluent comprising of potassium dichromate in deionised
water. The effects of the initial hexavalent chromium concentration, dose of biosorbent, and removal kinetics were explored. An
adsorbent dosage of 4 g/L was effective in complete removal of the metal ion, at pH 2.5, in 48 minutes. The kinetic process of
Cr(VI) adsorption onto potato peel powder was tested by applying pseudo-first-order and pseudo-second-order models as well as
the Elovich kinetic equation to correlate the experimental data and to determine the kinetic parameters. The adsorption data were
correlated by the Langmuir and Freundlich isotherms. A maximum monolayer adsorption capacity of 3.28 mg/g was calculated
using the Langmuir adsorption isotherm, suggesting a functional group limited adsorption process. The results confirmed that
potato peels are an effective biosorbent for the removal of hexavalent chromium from effluent.
Adsorption Studies of an Acid Dye From Aqueous Solution Using Lagerstroemia ...IJMER
The effectiveness of adsorption for acid dye removal from wastewaters has made it an ideal alternative to other expensive treatment options. The removal of acid Violet 4BS onto seeds of Lagerstroemia indica (LIS) from aqueous solutions was investigated using parameters such as contact time, pH, temperature, adsorbent doses, and initial dye concentration. Adsorption isotherms of dyes onto LIS were determined and correlated with common isotherm equations such as the Langmuir and
Freundlich models. It was found that the Langmuir isotherm appears to fit the isotherm data better than
the Freundlich isotherm. Parameters of the Langmuir and Freundlich isotherms were determined using adsorption data. The maximum removal of Acid Violet 4BS by the adsorbent was obtained at pH 2. The maximum percentage of dye removal (86.67%) was obtained at an initial dye concentration of 10mg/L with adsorbent dosage of 50 mg per 50 ml of dye solution. The adsorption kinetics of acid violet 4BS could be described by the pseudo-second order reaction model. The data obtained from adsorption
isotherms at different temperatures were used to calculate several thermo-dynamic quantities such as the
Gibbs energy (ΔG0), enthalpy (ΔH0), and entropy (ΔS
0) of adsorption. The adsorption process was found
to be spontaneous, exothermic and physical in nature. Locally available adsorbent LIS was found to have
a low cost and was promising for the removal of acid violet 4BS from aqueous solutions
While document and file sharing is increasing rapidly, 97% of organizations cite file sharing as a high risk for information loss, and 75% believe their organization is currently at risk for data loss.
A SEMI-BLIND WATERMARKING SCHEME FOR RGB IMAGE USING CURVELET TRANSFORMijfcstjournal
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eyes are not much sensitive to blue color. So the blue color plane of the cover image is used as embedding
domain. A bit planes method is also used, the most significant bit (MSB) plane of watermark image is used
as embedding information. Selected scale and orientation of the curvelet coefficients of the blue channel in
the cover image has been used for embedding the watermark information. All other 0-7 bit planes are used
as a key at the time of extraction. The results of the watermarking scheme have been analyzed by different
quality assessment metric such as PSNR, Correlation Coefficient (CC) and Mean Structure Similarity Index
Measure (MSSIM). The experimental results show that the proposed technique gives the good invisibility of
watermark, quality of extracted watermark and robustness against different attacks.
This is a guide to provide important information about selling your home during the winter of 2017. Contact Jessica Eve Morgan for a complimentary Home Evaluation. (646) 820-7855
A presentation about the services available to the construction industry from repair and restoration specialists Magicman, presented by Technical Adviser Louie Markwick.
Compliance Watcher introduction presentation-
Compliance Watcher helps in reducing non productive time of responsible teams by cutting down/ eliminating time spent on information gathering, compiling, processing, and reporting compliance status - resulting in avoiding of penalties and harassment.
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Chemo bio synthesis of silver nanoparticlesJagpreet Singh
Silver nanoparticles have a lot of ways of synthesis like physical and chemical
methods; some of these methods use a lot of chemical substances and are
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A very simple, highly selective and non-extractive spectrophotometric method for the trace amounts of palladium(II) has been developed. Pyridoxal thiosemicarbazone (PTSC) has been proposed as a new analytical reagent for the direct non-extractive spectrophotometric determination of palladium (II). The reagent reacts with palladium in acidic medium(pH 2.0, CH3COONa and Con. HCl ) to form a pale yellow coloured 1: 2 (M : L) complex. The reaction is instantaneous and the maximum absorption was obtained at 420 nm and remains stable for 2 hrs. The molar absorptivity and sandell’s sensitivity were found to be 1.63 x 104 L mol-1 cm-1 and 0.635 μg cm-2 respectively. Linear calibration graphs were obtained for 0.9- 10.0 μg/ml of palladium(II). The method is highly selective for palladium and successfully used for determination of palladium in various hydrogenation catalysts.
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Indigenized remote control interface card suitable for MAFI system CCR equipment. Compatible for IDM8000 CCR. Backplane mounted serial and TCP/Ethernet communication module for CCR remote access. IDM 8000 CCR remote control on serial and TCP protocol.
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Indigenized remote control interface card suitable for MAFI system CCR equipment. Compatible for IDM8000 CCR. Backplane mounted serial and TCP/Ethernet communication module for CCR remote access. IDM 8000 CCR remote control on serial and TCP protocol.
• Remote control: Parallel or serial interface
• Compatible with MAFI CCR system
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• Compatible with commercial and Defence aviation CCR system.
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New Analytical Technique For The Determination Of Mercury (II) By Synergistic Extractive Spectrophotometric Method With N'',N'''-Bis[(E)-(4-fluorophenyl)methylidene] Thiocarbonohydrazide
1. International Journal of Pharmaceutical Science Invention
ISSN (Online): 2319 – 6718, ISSN (Print): 2319 – 670X
www.ijpsi.org Volume 6 Issue 1 ‖ January 2017 ‖ PP. 50-62
www.ijpsi.org 50 | P a g e
New Analytical Technique For The Determination Of Mercury
(II) By Synergistic Extractive Spectrophotometric Method With
N'',N'''-Bis[(E)-(4-fluorophenyl)methylidene]
Thiocarbonohydrazide
Rekha A. Nalawadea,b
, Avinash M. Nalawadeb
, Arjun.N. Kokare a
, Sunil B.
Zanjea
, Mohan D. Jamdara
, Mansing A. Anusea
*
a
Analytical Chemistry Laboratory, Department of Chemistry, Shivaji University, Kolhapur 416004,
Maharashtra, India
b
Lal Bahadur Shastri College of Arts, Science and Commerce, Satara, 415002, Maharashtra, India.
Abstract: A new technique was developed for the extractive spectrophotometric determination of mercury (II)
by using newly synthesized chromogenic reagent N'',N'''-bis[(E)-(4-fluorophenyl)methylidene]
thiocarbonohydrazide bis-(4-fluoroPM)TCH. It forms yellow colored ternary complex with mercury(II) in
presence pyridine having composition 1:1:1 (M:Reagent:Py) in acidic pH range 1.7-3.7. The reagent is highly
sensitive and selective towards mercury(II). So spectrophotometric method of mercury(II) is found to be very
rapid, reliable and show synergistic effect. Absorption of colored organic layer in iso amyl acetate is measured
with reagent blank at λmax 375 nm. Pyridine showed synergistic effect with reagent by the adduct formation in
organic phase. Beer’s law was obeyed in the concentration range 0.25 to 3.5 µg mL-1
for mercury (II). Molar
absorptivity and sandell’s sensitivity values of mercury(II)-bis-(4-fluoroPM)TCH-Py complex are 0.50127x105
lit mol-1
cm-1
and 0.004 µg cm-2
, respectively. The selectivity of the method was checked by using various foreign
ions. The composition of the complex was determined by slope ratio method, mole ratio method and Job’s
method of continuous variation. The colour of ternary complex was stable for more than 12 h. Various factors
influencing on degree of comlexation are the effect of pH, reagent concentration, synergent concentration,
equilibrium time, solvent were determined. The method was applicable for determination of mercury(II) in
binary mixture, ternary mixture, ayurvedic sample, homoeopathic sample, industrial waste water, spiked water
and dental unit waste water.
Keywords: Synergenic extraction, Mercury (II), bis-(4-fluoroPM) TCH, Pyridine, ternary mixture
I. Introduction
The abundance of mercury in the earth crust is 0.067 ppm. Mercury is so volatile that it could be
exposed easily to human environment. It would cause a neurological damage and even result in death [1].
Mercury is also believed o be the most dangerous of all the metal contaminants which may be present in our
daily foods[2]. Compounds of mercury consumed in fish, cereals and other food stuffs have resulted in
numerous poisoning[3]. The acute mercury poisoning is “Minamata disease” which causes mental disturbance;
a loss of balance, speech, sight and hearing, difficult in swallowing and finally coma and death[4].The analysis
and monitoring of mercury in environmental, biological, industrial and food samples is extremely important
because of its high toxicity both in its organic and inorganic compounds[5] . The toxicity of mercury depends on
its chemical state[4].Inorganic mercury has a very high affinity for protein sulfhydryl groups, and accumulated
in the kidneys, whereas organic mercury has a greater affinity for brain. Elemental and inorganic mercury are found in
scientific instruments, electrical equipment, dental amalgams, felt making, disinfectants and enters the environment as
metallic, inorganic and organic mercury compounds through various industries like pulp and paper industry, chlor-
alkali plants,gold and silver mining, electrical energy, paints ,fungicides and pharmaceuticals[6]. Hence there
has been a growing interest to develop the analytical procedures for the determination of trace amounts of
mercury.Many sensitive instrumental techniques, such as spectrofluorimetry, X-ray fluorescence spectrometry,
neutron activation analysis, atomic absorption spectrometry, chemiluminescence, electrochemical analysis, and
other have been widely applied to the determination of mercury[7-11]. However, the spectrophotometric method
has still the advantage of its simplicity and accessibility, not needing expensive or complicated equipments. For
this reason, a wide variety of spectrophotometric methods for the determination of mercury have been reported
[12-17]. Each chromogenic system has its advantages and disadvantages with respect to sensitivity, selectivity
and analysis speed. Therefore, we have proposed synergistic, highly sensitive, simple and rapid method for
extraction and spectrophotometric determination of mercury(II) when compared with other spectrophotometric
methods[18-30](Table 1).
2. New Analytical Technique For The Determination Of Mercury (II) By Synergistic Extractive
www.ijpsi.org 51 | P a g e
II. Materials And Methods
2.1. Apparatus
All chemicals used were of analytical grade, from S. d. Fine. Lab Junction digital spectrophotometer
model LJ-1306 using 1 cm quartz cell was used to obtain optical density. A model LI-120 Elico digital pH
meter with combined glass electrode was used for measurement of pH. Glasswares were washed with chromic
acid followed by double distilled water.
2.2. Standard mercury(II) solution and solution of other cations and anions
A 1.353 g of mercuric chloride,(HgCl2 Merck) was dissolved in water and diluted to 1 lit to make stock
solution of mercury(II) (1 mg mL−1
).It was standardized by a comlpexometric titration [31]. Double distilled
water was used throughout the experiment. Salts of different cations and anions were dissolved in water or dil.
HCl/H2SO4/HNO3 to make their solutions[32]. Different synthetic mixtures containing mercury (II) were
prepared by combining with commonly associated metal ions in definite composition [33].
2.3.Synthesis of N'',N'''-bis[(E)-(4-fluorophenyl)methylidene]thiocarbonohydrazide [bis-(4-fluoroPM)TCH
]It is two step synthesis process.
Preparation of thiocarbohydrazide (TCH) – It is synthesized by various methods [34-37]. We have followed the
method of Li. Zheng., X. Feng, Y. Zhao.
Two moles of hydrazine hydrate were refluxed for two hours in an aqueous medium with one mole of carbon
disulphide to give thiocarbohydrazide (TCH).
NH 2 N H 2
S
S
+
Heat
Water
S
N H N H
NH 2
N H 2 +2 SH 2
TCH
b. One mole of TCH was refluxed with two moles of p- fluoro benzaldehyde in alcohol as a solvent and glacial
acetic acid as a catalyst to give N'',N'''-bis[(E)-(4-fluorophenyl)methylidene] thiocarbonohydrazide [bis-(4-
fluoroPM)TCH] [38].
F C H N N H
S
F C H O
FC HNN H
NH2
N H
S
N H2
N H 2+
g la c ia l a c e tic a c id
[bis-(4-fluoroPM)TCH]
Purity of analytical reagent was tested by melting point, TLC, IR and NMR. A 0.01 M stock solution of bis-(4-
fluoroPM)TCH was prepared by dissolving 0.299 g in a 100 cm3
of amyl acetate.
2.4. Recommended procedure
Mercury(II) (1ml of 25 μg mL−1
) solution was taken in 25 mL calibrated flasks and pH adjusted to 3.0
with dil hydrochloric acid or sodium hydroxide was used. The solution was transferred into 125 mL separatory
funnel, followed by addition of 1ml of 0.002M bis-(4-fluoroPM)TCH, 4 ml amyl acetate, 5.0 mL of 0.5 M
pyridine in amyl acetate. The two phases were equilibrated to 5 min. The yellow coloured organic extract was
collected over anhydrous Na2SO4 to remove the traces of water. Then solution was transferred into 10 mL
standard volumetric flask and made up to the mark with amyl acetate if necessary. The absorbance of the
complex was measured at λmax 375 nm against a reagent blank prepared in the same way, without addition of
mercury(II). Unknown amount of mercury(II) was determined from the calibration graph prepared in the same
manner.
III. Results And Discussion
3.1. Absorption spectra and spectral characteristics of coloured complex
Faint yellow coloured ternary complex was formed by mercury(II) with bis-(4-fluoroPM)TCH having
proportion 1:1:1 (M :Reagent :Py), in the presence of pyridine as an auxiliary ligand. It was then extracted into
amyl acetate at pH 3.0. The absorption spectra of mercury(II)-bis-(4-fluoroPM)TCH-Py complex in amyl
acetate was studied over the wavelength range 300–800 nm. The coloured mercury(II)-bis-(4-fluoroPM)TCH-
3. New Analytical Technique For The Determination Of Mercury (II) By Synergistic Extractive
www.ijpsi.org 52 | P a g e
Py complex was showed maxima at λmax 375 nm in amyl acetate, while reagent showed maxima at λmax 365
nm.[Fig. 1] Complex was stable for more than 12 h. The optimum conditions for the effective extraction of
mercury(II) was established by studying the effect of pH, reagent concentration, pyridine concentration, choice
of solvent, equilibrium time and interference of various diverse ions.
3.2. Effect of pH
The absorbance of mercury(II)-bis-(4-fluoroPM)TCH-Py complex was studied for wide range of pH
from 1 to 10 by using 0.1N NaOH and 0.1N HCl solution. The extraction of mercury(II) was carried out with
the bis-(4-fluoroPM)TCH-Py in presence and absence of pyridine. The study showed that the maximum
absorbance was shown in the pH range 2.5-4.5 in the absence of pyridine for mercury(II)-bis-(4-
fluoroPM)TCH-Py complex. However, in the presence of pyridine there was increase in the absorbance and
shifting in the pH range to more acidic medium1.7-3.7, showed synergistic effect on absorption
mercury(II)-bis-(4-fluoroPM)TCH-Py complex [Fig. 2]. Further extraction was carried out at pH 3.
3.3. Influence of solvents on determination of mercury(II)
Mercury –bis-(4-fluoroPM)TCH-py complex was found to be insoluble in aqueous medium. However it
is very soluble in non-polar solvents. The percentage efficiency of the complex in various solvent is shown in
decreasing order as iso amyl acetate (99.9). > methyl iso butylketone (95.33) > xylene (91.61) > benzene
(89.15 ) > dichloromethane (72.0 ) > toluene (65.4) > chloroform (53.0) > amyl alcohol (45.7 ) > butyl
alcohol (28.0 ) >1,2- dichloro ethane (4.67) > carbon tetrachloride (2.8).
As percentage efficiency of the mercury(II)-bis-(4-fluoroPM)TCH-Py complex in iso amyl acetate is maximum
among these solvents, iso amyl acetate was use for further extraction.
3.4. Effect of [bis(4-fluoroPM)TCH]concentration
Extraction and spectrophotometric determination of mercury(II)-bis-(4-fluoroPM)TCH-Py complex
was effected by concentration of chelating reagent bis-(4-fluoroPM)TCH. The concentrations of bis-(4-
fluoroPM)TCH in amyl acetate were varied from the range 1 x10-5
to 10 x10-4
mol L−1
and were added
to a 1 ml of 25 μg mL−1
mercury(II) ion solution in the absence of pyridine and absorbance was measured
according to the recommended procedure. For maximum absorbance of complex 1.5 mL of 0.001 mol L−1
reagent was used. However in presence of pyridine only 0.3 ml of 0.002 mol L−1
reagent was sufficient for full
color development. In order to ensure the complete complexation, 1.0 mL of 0.002 mol L−1
reagent was
recommended. In the absence of pyridine reagent concentration was 1.5x10-4
M and in presence of pyridine
reagent concentration was 6x10-5
M. Requirement of less concentration of reagent in presence of pyridine
showed synergistic effect on the extraction. Excess of reagent does not affect absorbance of the complex upto,
2.0 mL of 0.002 mol L−1
concentration of reagent. Then there was decrease in absorbance with more increase
in concentration [Fig.3].
3.5. Effect of equilibrium time
The equilibrium time was varied from 0.25 to 60 min in the absence and presence of pyridine. The
minimum shaking time of 7 min of mercury(II)-bis-(4-fluoroPM)TCH-Py complex was investigated for full color
development in the absence of pyridine. In the presence of pyridine absorbance was increased and required
minimum of 3 min shaking time for full color development. Prolonged shaking time has no adverse effect on the
absorbance of mercury(II) in the presence of pyridine. Hence, a shaking time of 5 min was recommended for
further study.
3.6. Effect of concentration of pyridine (Auxillary ligand)
Mercury(II)-bis-(4-fluoroPM)TCH complex was affected by pyridine concentration. Solution of Hg(II)
(1 ml of 25 μg mL−1
) and 1 ml of 0.002 mol L−1
of bis-(4-fluoroPM)TCH was equilibrated with 0 to 5.0 ml of
0.5 mol L−1
concentration range of pyridine. The mercury(II)-bis-(4-fluoroPM)TCH complex was decomposed
after 4 h in the absence of pyridine. However, absorbance of mercury(II)-bis-(4-fluoroPM)TCH complex
increases with pyridine concentration and remains constant above 3.0 mL of 0.5 mol L−1
pyridine for 12 h. This
indicates that the absorbance of mercury(II)-bis-(4-fluoroPM)TCH complex was increased by the formation of
an adduct with pyridine. Therefore, 5.0 mL of 0.5 mol L−1
pyridine was used in experimental study.
3.7. Effect of stability of complex
Mercury-bis-(4-fluoroPM)TCH-Py complex showed stable absorbance for more than 12 h in presence
of pyridine in amyl acetate solution, while in the absence of pyridine absorbance was found to be low and
decreased after 4 h. Therefore it was recommended that study of mercury(II)-bis-(4-fluoroPM)TCH-Py complex
was carried out in presence of pyridine.
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3.8. Determination molar extinction coefficient and sensitivity
Mercury-bis-(4-fluoroPM)TCH-Py complex was obeyed Beer’s law over conc range 0.25 to 3.5 μg
mL−1
. The precision and accuracy of the proposed method was ascertained from the absorbance values of the
actual determinations of five replicates of fixed amounts of the mercury(II) samples. To determine the accuracy
of the proposed method; different amount of samples containing mercury(II) were taken within the optimum
Beer’s range limits and analyzed by the recommended procedure. The molar extinction coefficient was
evaluated from slope of curve was 5.0127 x104
lit mol-1
cm-1
and Sandell’s sensitivity values of complex was
0.004 μg / cm2
.
3.9 Ringbom’s plot for complex
The optimum Beer’s range was evaluated by Ringbom’s plot. It is sigmoid shape with linear segment at
intermediate concentration values in the range of 0.5- 3.0 μg mL−1
for mercury(II).
3.10 Determination of metal:ligand ratio
The probable composition of the mercury(II)-bis-(4-fluoroPM)TCH-Py complex was ascertained by Job’s plot,
mole ratio method and slope ratio method.
3.10.1. Job’s plot
Mercury(II), bis-(4-fluoroPM)TCH and pyridine solutions were taken in equimolar (2.494x10-4
mol L-
1
) proportions. Different aliquots(0.2-1.8) of equimolar mercury(II) solution was taken in 25 mL calibrated
flask and pH was adjusted to 3.0. The solution was transferred into 125 mL separatory funnel followed by
different aliquots of (1.8-2.0) equimolar reagent in each flask, keeping the total volume of metal and ligand
solution constant at 2.0 mL. It was followed by 5.0mL of pyridine and amyl acetate, keeping the total volume of
organic phase to be 10 mL. After equilibrium, the absorbances of the each organic phases were recorded at
375 nm, against the corresponding reagent blanks. The same procedure was described under the absence of
pyridine. [Fig. 4]
3.10.2. Mole ratio method:
In this method also mercury(II), bis-(4-fluoroPM)TCH and pyridine solutions were taken in equimolar
(2.494x10-4
mol L-1
) proportions To a equimolar (2.494x10-4
mol L-1
) solutions of 1 ml of bis-(4-fluoroPM)TCH
and 5.0 mL of pyridine different aliquots(0.2-1.8) of mercury(II) solution with pH 3.0 containing were added.
Then 4.0 mL of iso amyl acetate was added to each of these solutions to keep the final volume of organic phase
10 mL. The absorbances of the organic phases were recorded at 375 nm. The similar procedure was followed
for the absence of pyridine. A plot between the absorbance versus number of moles of the ligand per mole of the
metal ion is shown in Fig. 5
3.10.3 Slope ratio method :
Mercury(II) (1ml of 25 μg mL-1
) solution having pH 4.0 which was other than selected pH was taken
in a 25ml volumetric flask. Different aliquots (0.1-1.7ml) of 0.002 mol / lit of bis-(4-fluoroPM)TCH in iso
amyl acetate and 5.0 mL of 0.5 mol L-1
pyridine and then required volumes of amyl acetate were added to keep
final volumes of each organic phase 10.0 mL. The optical density of the organic phase was recorded at 375 nm
against reagent blank. The composition of the mercury(II)-bis-(4-fluoroPM)TCH-Py complex was ascertained
by plotting the graph of log D[Hg (II)] against log C[bis(4-fluoroPM)TCH]at fixed 0.5 mol L-1
pyridine concentration and
log D[Hg (II)] against log C[Pyridine] at fixed reagent concentration at pH 4.0. Similar procedure was repeated at pH
5.0.The plots were linear having the slopes 0.95 and 0.93 at pH 4.0 and pH 5.0, respectively with fixed pyridine
concentration (Fig. 4.11) and 0.59 and 0.62 at pH 4.0 and pH 5.0, respectively with fixed reagent concentration
(4.12). The composition of extracted species (Metal:Reagent:Pyridine) was 1:1:1. The following chemical
reactions are took place and probable coloured extracted species M:L:Py is
N
H
N
H
S
N
H
N
H
N
H
N
SH
N
H
N
H
F F F F
Tautomerization
(1)bis-(4-fluoroPM)TCH(keto form bis-(4-fluoroPM)TCH (enol form)
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N
H
N
SH
N
H
N
H
F F
dissociation
N
H
N
S-
N
H
N
H
F F
+ H+
(2)bis-(4-fluoroPM)TCH (enol form)
Anionic form of bis-(4-fluoroPM)TCH
(3) Hydrolysis of HgCl2 to Hg(OH)Cl occurs at pH 3.0 [39].
HgCl2 + 3H2O
Hydrolysis
[Hg(OH)Cl(H2O)2] + H+
+ Cl-
(4)
Probable structure of mercury-[bis-(4-fluoroPM)TCH]-Py complex/adduct
3.11Interference study
Under the optimum conditions cited above with 25 μg /ml a systematic study of the effect of foreign
cations and anions ions was undertaken(Table 4.4). The selectivity of the method was eliminated by using
suitable masking agents for cations.
IV. Applications
4.1. Separation of mercury (II) from gold(III)
When gold comes into contact with mercury, the two substances mix to form a compound called
amalgam. Gold amalgam is simply an alloy of gold and mercury. Bis-(4-fluoroPM)TCH reagent is used for the
separation and determination of mercury(II) from gold(III) by its extraction given in recommended procedure.
Mercury(II) was separated from gold(III) by its extraction with recommended procedure without using
masking agent. Under optimized conditions gold(III) remained quantitatively in the aqueous phase. The aqueous
phase was evaporated to moist dryness by treating with 2.0 mL conc HNO3 followed by 2 to 3 ml of conc HCl.
The residue was dissolved in dil HCl and diluted to appropriate volume. Gold(III) ions from aqueous phase
were determined by standard method [40].The absorbance of mercury(II)-bis-(4-fluoroPM)TCH-Py complex
was determined spectrophotometrically at 375 nm against reagent blank.
4.2. Separation of mercury(II) from associated metal ions
By following the recommended procedure and using bis-(4-fluoroPM)TCH mercury(II) was also
separated from Fe(III), Ni(II), Bi(III), Cr(III), Al(III), Zn(II), Cd(II), Pb(II), Sn(II), Sn(IV),Se(IV), Te(IV). But
Fe(III), Ni(II), Bi(III), Cr(III), Al(III), Zn(II), Cd(II), Pb(II), Sn(II), Sn(IV) ions were interfered with extraction
of mercury(II). So Ni(II), Cd(II) masked with 1.0 mg thiocynate; Fe(III), Pb(II),Zn(II)and Cr(III) masked with
5 mg tartarate; each Bi(III), Al(III) masked with 0.03 mg citrate; Sn(II) and Sn(IV) masked with 5 mg oxalate.
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The masked metal ions as an anionic complex were remained in the aqueous phase quantitatively and were
subsequently demasked by treating with 2.0 mL of conc HClO4 and followed by 1 ml conc HCl. The solution was
evaporated to moist dryness. Obtained residue was dissolved in water, diluted to appropriate volume and metal
ions were determined spectrophotometrically by standard methods [32,33,41]. Mercury(II) was separated from
Se(IV) and Te(IV) by using recommended procedure. Under optimum conditions Se(IV) and Te(IV) were
remained in the aqueous phase quantitatively. The aqueous phase was evaporated to moist dryness by treating
with 5.0 mL conc HNO3 followed by 1ml conc HCl. The residue was dissolved in water and diluted to
appropriate volume. The added metal ions were determined spectrophotometrically by standard methods
[42,43]. The absorbance of mercury(II)-[bis(4-fluoroPM)TCH]-Py complex from organic phase was
measured at 375 nm against reagent blank (Table 3).
4.3. Determination of mercury(II) from synthetic mixtures
By using 25 μg mL-1
of mercury(II) and known concentration of associated metal ions several synthetic
mixtures of varying compositions were prepared. It was followed by suitable masking agent if required. The
extracted mercury(II) was analyzed by employing the bis-(4-fluoroPM)TCH by recommended procedure. The results
obtained were same as the amount added (Table 4).
4.4Analysis of mercury(II) from ayurvedic samples
The developed method was applied for the determination of mercury(II) in ayurvedic samples such as
Echabhedi and Ekangveer Rasa. 1 tablet of a known weight of sample was dissolved in required volume of aqua
regia followed by treatment with 2.0mL of conc HClO4. The solution was evaporated to moist dryness. Obtained
residue was dissolved in hot dil HCl and filtered through Whatmann filter paper No. 1. The filtrate was diluted to
required volume with water to obtain results within optimum Beer’s range. An aliquot of mercury(II) content in
solution was determined by the recommended procedure. The results were in good agreement with those obtained by
atomic absorption spectroscopy (Table 5).
4.5Analysis of mercury (II) from homeopathic pharmaceuticals
An aliquot (5.0 mL) of each homeopathic pharmaceutical sample was used for determination of Hg(II) and
followed by the recommended procedure. The results of analysis was found to be in excellent agreement with those
obtained by AAS (Table 6).
4.6 Analysis of mercury(II) from industrial waste water samples
Each waste water sample (100.0 mL) was evaporated almost to dryness. The residue was dissolved in
5.0 mL of conc nitric acid and 20.0 mLof water, boiled and filtered through Whatmann filter paper No. 1. The
filtrate was diluted to required volume with water. An aliquot (5ml) of sample was taken into 25 ml calibration
flask and mercury content was determined by recommended spectrophotometric method. The results of analysis
were confirmed by AAS (Table 7).
4.7 Determination of mercury (II) in spiked water samples
The water samples were spiked with several known amounts of mercury(II). The analytical determination of
mercury was carried out by recommended spectrophotometric method.The results of analysis were checked by
AAS (Table 8)
4.8 Determination of mercury (II) in dental waste water samples
Mercury(II) in dental-unit waste water samples were collected from dental clinics at Kolhapur city.
Each sample (100.0 mL) was evaporated almost to dryness. The residue was dissolved in 5.0 mL of conc nitric
acid and 20.0 mLof water, boiled and filtered through Whatmann filter paper No. 1. The filtrate was diluted to
required volume with water. An aliquot (5ml) of sample was transferred into 25 ml calibration flask and
mercury(II) content was determined by recommended method. The results of analysis were compared with AAS
(Table 9).
V. Conclusion
A simple, synergistic, rapid, sensitive spectrophotometric method was proposed for determination of
trace amount of mercury(II) in binary, synthetic mixtures, and various real samples with satisfactory results.
The newly synthesized reagent bis-(4-fluoroPM)TCH has been proved to be highly sensitive for solvent
extraction and spectrophotometric determination of mercury(II) when compared to other spectrophotometric
methods (Table1).Therefore very less concentration of mercury(II)[25 μg mL-1
] can be determined by using this
reagent with very low reagent concentration in a single stage extraction procedure. The extracted complex is
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stable for more than 12 h in presence of pyridine. The selectivity was enhanced by the use of suitable masking
agents.
Abbreviations
bis-(4-fluoroPM)TCH N'',N'''-bis[(E)-(4-fluorophenyl)methylidene]
thiocarbonohydrazide
4’-chloro PTPT 1-(4’-chlorophenyl)-4,4,6-trimethyl(1H,4H)-2-
pyrimidine thiol
2’,4’-dinitro APTPT 1-(2’,4’-dinitro aminophenyl)-4,4,6-trimethyl-1,4-
dihydropyrimidine-2-thiol
DMG Dimethylglyoxime
PAR 4-(2-Pyridylazo) resorcinol
Py Pyridine
Table 1 Comparison of proposed method with reported solvent extraction and spectrophotometric methods for
determination of mercury(II).
Reagent λmax
nm
Acidity/
pH
Beer’s law Molar
absorptivity
Remarks Ref. No.
N'',N'''-bis[(E)-(4-
fluorophenyl)methylidene]
thiocarbonohydrazide [bis-(4-
fluoroPM)TCH]
375 1.7-3.7 2.5-30 0.501x105
*Simple
*Highly sensitive
*Rapid
P.M.
2-mercaptobenzothiazole (MBT) 320 10.00 1.0x 10-7
1.0x 10-5
- *Use of nonionic
surfactant Triton X
100
*Buffer solution is
required to adjust
pH
18
Isonitriso p-isopropyl
Acetophenone Phenyl
Hydrazone (HIPAPH)
395 7-11 1.0 to 20 2.67x10-3
*Stiochiometry 1:2
*Hg(II) was
determined from
real samples
19
6-hydroxy-3-(2-oxoindolin-
3-ylideneamino)-2-
thioxo-2H-1,3-thiazin-4(3H)-one,
366,
505
4.0-6.0 0.2–2.0 4×104
*Excess of
chromogenic reagent
*Hg(II) was
determined from
real samples
20
o-carboxy phenyl diazoamino
p-azobenzene
540 .08-8.0 2.22×105
*Excess of
chromogenic reagent
*Surfactant used
was Triton X 100
21
4,4'-
(dimethylamino)thiobenzophenone
575 1-6 12-140 1.7×104
*Sensitive
*Hg(II) was
determined from
water samples
* High reagent
concentration
required
22
6-mercaptopurine 315 5-8 002-.048 0.26x10-6
*Wide Beer’s range.
*Buffer solution was
required to adjust
pH. *surfactants are
used
23
Thiacrown ether and Bromocresol
Green
420 - - - *Less sensitivity
*Interference from.
Cu+2,
Cd2+
and Ag+
.
*Time-consuming
24
Hydentoin,5‐ amino1,3,4‐ thiadizole
‐ 2‐ thiol (HTT)
490 6.0-8.0 2.2 6.45x 104
*Reagent was
sensitive
* Narrow Beer’s
range.
25
2-(2-thiazolylazo)-p-cresol) 500 9.5 10 5.7x104
Surfactants are used 26
Anthrone phenylhydrazone (APH) 367 7 0.81-8.14 1.267×104
*Less stability of
complex. *Buffer
solution was
required to adjust
pH.
27
Diphenylthiocarbazone (dithizone) 488 0.18–
1.8
0.1-25 2.5 × 104
*Use of surfactants
*Reagent was
28
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sensitive.
2-Acetylpyridine thiosemicarbazone
(APT)
351 6 0.24-2.40 5.4x104
*Less stability of
complex *Buffer
solution was
required to adjust
pH.
29
4-Hydroxy 3, 5-dimethoxy
benzaldehyde 4-hydroxy
benzoylhydrazone (HDMBHBH)
420 4 0.30-3.09 4.56x104
*Complex was
stable in micellar
solution.
30
Table 2 Effect of diverse ions for the determination of 25 μg mL-1
mercury(II) with bis(4-fluoroPM)TCH and
pyridine complex. (relative error ± 2%)
Amount of foreign ion added mg Tolerance limit, mg
NO3
-
, NO2
-
25
Oxalate, salicylate, F-
10
Tartarate 5
SCN-
1
Citrate, Ag(I) 0.03
c
Zn(II) 0.8
Ga(III), Y(III), c
Pb(II) , b
Fe+
(III), b
Ni(II) 0.5
b
Cr(III),b
Cr(VI), Te(IV), d
Bi(III), d
Pd(II), b
Cd(II) 0.1
e
Sn(II) , e
Sn(IV), Au(III), a
Pt(IV), b
Co(II) 0.05
d
Sb(III), b
Mo(VI) 0.08
d
Al(III) 0.3
b
Mn(II), b
Mn(VII)
Se(IV)
0.01
0.4
a
0.01 mg of S2O3
2- d
0.03 mg of citrate
b
1.0 mg of SCN- e
10 mg of oxalate
c
5 mg of tartarate
Table 3. Separation of mercury(II) from associated metal ions
a
Masked with 10 mg of oxalate d
Masked with 0.03 mg of citrate
b
Masked with 1.0 mg of SCN- c
Masked with 5 mg of tartarate
* Average of five determinations
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Table 4. Determination of mercury(II) in a synthetic mixtures
Composition, μg Average % Recovery* R.S.D. %
Hg(II), 25; Cr(III)b
, 100; Cd(III)b
, 100 97.2 1.82
Hg (II), 25; Cr(III)b
, 100; Pb(II)c
, 300 97.1 1.92
Hg (II), 25; Sn(II)a
, 50; Fe(III)b
, 100 97.7 0.70
Hg (II), 25; Sn(IV)a
, 50; Fe(III)b
, 100 97.3 1.40
Hg (II), 25; Zn(II)c
, 100; Cd(II)b
, 100 97.4 1.52
Hg (II), 25; Sb(III)d
, 100; Pb(II)c
, 100 97.2 1.82
Hg (II), 25; Bi(III)d
, 400; Pb(II)c
, 100 97.2 1.82
Hg (II), 25; Al(III)d
, 100; Zn(II), 100 97.2 1.82
Hg (II), 25; Fe(III)b
, 400; Al(III)d
, 100 97.1 1.92
Hg (II), 25; Al(III)d
, 100; Cd(III)b
, 100 97.2 1.82
Hg(II),25; Se(IV), 400; Te(IV),100 97.1 1.92
a
Masked with 10 mg of oxalate c
Masked with 5 mg of tartarate
d
Masked with 0.03 mg of citrate b
Masked with 0.8 mg of SCN-
*
Average of five determinations
Table 5. Determination of mercury(II) from ayurvedic samples
Name of sample Certified Values
of Hg(II) mg
Amount of Hg(II) found*
(mg/250 gm)
R.S.D.,
%
Proposed method AAS method 1.36
Echabhedi 25.0 25.1 25.0 3.98
Ekangveer Rasa2
Feb
; Sna
; Pbc
66 66.2 66.0 3.78
* Average of five determinations
a
Masked with 10 mg of oxalate c
Masked with 5 mg of tartarate
b
Masked with 1.0 mg of SCN-
Table 6. Determination of mercury(II) from homoeopathic samples
Homoeopathic medicine Amount Added
(μg/ml)
Amount of Hg(II) found*
(μg/ml)
R.S.D.,
%
Proposed method AAS method
Mer cor Q 0.100 0.116 0.115 1.36
Mer sol Q 0.100 1.108 0.108 1.20
* Average of five determinations
Table 7. Determination of mercury(II) from Industrial Waste water samples
Water sample Amount of Hg(II) found*(μg/ml) R.S.D., %
AAS method Proposed method
Sample 1 0.147 0.148 1.36
Sample 2 0.118 0.120 1.20
* Average of five determinations
Table 8. Determination of mercury(II) from Spiked water samples
Water samples Hg(II) Added
(μg/ml)
Amount of Hg(II) found*(μg/ml) R.S.D., %
Proposed method AAS method
Tap water 3.0 3.05 3.05 1.40
5.0 5.06 5.08 1.66
7.0 7.08 7.08 1.20
Lab water 0.0 20.1 20.1 1.10
100 120.2 120.1 1.35
500 500.2 500.2 1.36
* Average of five determinations
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Table 9 Determination of mercury(II) from Dental waste water samples
Water sample Hg(II) Added
(μg/ml)
Amount of Hg(II) found*
(μg/ml)
R.S.D.,
%
AAS method Proposed
method
Dental waste water sample 1 -a
2.22 2.22 1.36
2.0 a
4.22 4.24 1.45
4.0 a
4.26 6.26 1.40
Dental waste water sample 2 - a
3.57 3.57 1.20
1.00 a
4.60 4.60 1.08
3.00 a
6.60 6.61 1.22
* Average of five determinations
a
Masked with 0.01 mg of S2O3
-2
Fig. 1
(A) The spectra of bis-(4-fluoroPM)TCH in iso-amyl acetate :
(bis-(4-fluoroPM)TCH = 1.0 mL of 0.002 mol L-1
; λmax = 365 nm
(B) The spectra of Hg(II)-bis-(4-fluoroPM)TCH-Py complex
Hg(II) = 25 μg mL-1
; bis-(4-fluoroPM)TCH = 1.0 mL of 0.002 mol L-1
; λmax = 375 nm
Fig. 2
A]Influence of H+
ions conc on the extraction Hg(II)-bis-(4-fluoroPM)TCH
complex: (without pyridine)
Hg (II) = 25 μg mL-1
; [bis(4-fluoroPM)TCH]-= 1.0 mL of 0.002 mol L-1
;
pH =1 to 10; λmax = 375 nm
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B]Influence of H+ ions conc on the extraction mercury(II)-bis-(4-
fluoroPM)TCH-Py complex: (with pyridine)
Hg (II) = 25 μg mL-1
; [bis(4-fluoroPM)TCH]-= 2.0 mL of 0.002 mol L-1
; pyridine =
5.0 mL of 0.5 mol L-1
pH =1 to 10; λmax = 375 nm
Fig.3.
(A)Effect of reagent conc. on extraction of mercury(II)-bis-(4-fluoroPM)TCH-Py
complex:
Hg (II) =25 μg/ mL pH =3.0;
bis-(4-fluoroPM)TCH = 0.1-5.0 mL of 0.002 mol L-
Pyridine = 5.0 mL of 0.5 mol L-1
;
Equilibrium time = 5 min; λmax = 375 nm
(B) Effect of reagent conc. on extraction of mercury(II)-bis-(4-fluoroPM)TCH complex
in absence of pyridine:
Hg (II) = 25 μg/ mL; pH =3.0,
bis-(4-fluoroPM)TCH = 0.1-10 mL of 0.001 mol L-1
Equlibrium time = 7 min;
λmax = 375 nm
Fig 4.
Job’s plot
Hg(II) = 0.2 to 1.8 mL of 2.494 x 10-4
mol L-1
,
bis-(4-fluoroPM)TCH = 1.8 to 0.2 mL of 2.494 x 10-4
mol L-1
;
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pyridine = 5.0 mL of 2.494 x 10-4
mol L-1
; pH = 3.0;
Equilibrium time = 5 min; λmax = 375 nm
Fig. 5
Mole ratio method
Hg (II) = 0.2 to1.8 mL of 2.494 x 10-4
mol L-1
;
bis-(4-fluoroPM)TCH = 1.0 mL of 2.494 x 10-4
mol L-1
;
pyridine = 5.0 ml of 2.494 x 10-4
mol L-1
;
pH = 3.0 ; shaking time = 5 min; λmax = 375 nm
Fig. 6
Slope ratio method: [Fixed pyridine concentration]
Hg (II) = 25μg mL-1
; pyridine = 5.0 mL of 0.5 mol L-1
; pH = 3.0 and 5.0;
bis-(4-fluoroPM)TCH = 2 x 10-5
to 34 x 10-5
mol L-1
;
shaking time = 5 min; λmax = 375 nm
Fig. 7.
Slope ratio method: [Fixed reagent concentration]
Hg (II) = 25 μg mL-1
; pyridine = 5.0 x 10-3
to 175 x 10-3
mol L-1
;
bis-(4-fluoroPM)TCH = 1 ml 0.002 mol L-1
(fixed concentration)
pH = 3.0 and 5.0; shaking time = 5 min; λmax = 375 nm;
13. New Analytical Technique For The Determination Of Mercury (II) By Synergistic Extractive
www.ijpsi.org 62 | P a g e
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