Method validation on iron determination by spectrophotometric method in aqueous medium

790-796This paper deals with the validation of a method for the determination of iron in spectrophotometric method in aqueous medium. The method is based on complex formation of iron with thioglycolic acid in alkaline medium in presence of a masking agent to produce a red purple chelate that has an absorption maximum at 535 nm wavelength. Beer-Lambert law is obeyed and linear calibration curves are obtained for the concentration range of iron from 0.1 mg/L to 30 mg/L. The reaction is found to be spontaneous in alkaline medium. The limit of detection and limit of quantification for the developed method are 0.0108 and 0.0345, respectively. Effect of different parameters like molar ratio of iron to different reagents and interferences, effect of time and effect of temperature of this method of determination have been studied. It is found that this method is moderately sensitive and has been successfully applied for the determination of iron(III) in different fields like ceramic materials, clay, sand, glass, stone, soil, water, and any inorganic iron containing compound or alloys. A comparison report is made for Chevron gas field waste material and Certified Reference Material of iron, which is done by atomic absorption and UV-visible spectroscopy techniques and found to be comparable

Method validation on iron determination by spectrophotometric method in aqueous medium

This paper deals with the validation of a method for the determination of iron in spectrophotometric method in aqueous medium. The method is based on complex formation of iron with thioglycolic acid (TGA) in alkaline medium in presence of a masking agent to produce a red purple chelate that has an absorption maximum at 535 nm wavelength. Beer’s-Lambert’s law is obeyed and linear calibration curves were obtained for the concentration range of iron from 0.1 mg/L to 30 mg/L. The reaction is found to be spontaneous in alkaline medium. The limit of detection (LOD) and limit of quantification (LOQ) for the developed method are 0.0108 and 0.0345 respectively. Effect of different parameters like molar ratio of iron to different reagents and interferences, effect of time and effect of temperature of this method of determination were studied. It is found that this method is moderately sensitive and has been successfully applied for the determination of iron (III) in different fields like ceramic materials, clay, sand, glass, stone, soil, water, and any inorganic iron containing compound or alloys. A comparison report is made for Chevron gas field waste material and Certified Reference Material (CRM) of iron, which was done by Atomic Absorption Spectrophotometer (AAS) and Ultraviolet-visible (UV-Vis) spectrophotometer and found to be comparable

Fabrication of Ferrous Sulfate from Waste Like Condensed Milk Containing Can and its Characterization

Ferrous sulfate is usually produced from the spent pickling liquor when the metal sheets are pickled in the processing of steel. In the present work ferrous sulfate was prepared by simple acid leaching method by using waste condensed milk can as a raw material. This can contains around 87 percent of iron which was successfully converted to greenish crystals of ferrous sulfate by simple acid leaching followed by crystallization. The process parameters like concentration of acid, molar ratio of iron to acid, period of reaction,effect of temperature and effect of occasional stirringwere optimized. Nearly 98% iron was leached out from iron containing can and converted to ferrous sulfate. The product was characterized by chemical analysis, thermo gravimetric analysis and X-ray diffraction analysis. On chemical analysis it was found that the produced product is highly pure, nearly 97 percent. According to the DSC/TGA studies, it is found that the prepared sample is hexahydrate. From X-ray diffraction pattern, it was confirmed that the prepared sample is ferrous sulfate with melanterite phase and have monoclinic crystal structure. Ferrous sulfate is usually produced from the spent pickling liquor when the metal sheets are pickled in the processing of steel. In the present work ferrous sulfate was prepared by simple acid leaching method by using waste condensed milk can as a raw material. This can contains around 87 percent of iron which was successfully converted to greenish crystals of ferrous sulfate by simple acid leaching followed by crystallization. The process parameters like concentration of acid, molar ratio of iron to acid, period of reaction,effect of temperature and effect of occasional stirringwere optimized. Nearly 98% iron was leached out from iron containing can and converted to ferrous sulfate. The product was characterized by chemical analysis, thermo gravimetric analysis and X-ray diffraction analysis. On chemical analysis it was found that the produced product is highly pure, nearly 97 percent. According to the DSC/TGA studies, it is found that the prepared sample is hexahydrate. From X-ray diffraction pattern, it was confirmed that the prepared sample is ferrous sulfate with melanterite phase and have monoclinic crystal structure

Effect of metal ions on structural, morphological and optical properties of nano-crystallite spinel cobalt-aluminate (CoAl2O4)

The bright blue nano crystallite cobalt aluminate (CoAl2O4) was synthesized by sol–gel method using a mixture of chelating agent of glycerol and citric acid. The effects of changing (0.05, 0.075, 0.10, 0.25, 0.50, and 0.75 mol/L) metal ion concentration on the structural, morphological and color properties of synthesized CoAl2O4 were characterized by using X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), Nanoparticle size analyzer, Simultaneous Thermal Analyzer (STA), UV–vis absorption spectroscopy, and CIE-LAB colorimetric analysis. From the X-ray peak profile analysis, the crystallite size was measured by Debye-Scherrer (D-S) equation, and three different models presenting average crystallite sizes between 88.3 and 125.4 nm.The average lattice strain, dislocation density, lattice constant, cell volume, and zeta potential were between 0.00021 and 0.0058, (1.73 to 12.8) × 1014 (lines/m2), 8.10658 to 8.11181 Å, 533.60 to 533.81 Å3, −56.4 to − 63.5 mV, respectively. Using UV–vis absorption spectroscopy, the band gap was calculated from Kubelka-Munk method, and the values of band gap increasing from 1.82 to 1.84 eV, respectively. The reflectance spectra and the CIE-L*a*b* values of cobalt aluminate is also measured which confirmed the formation of blue nano crystallite cobalt aluminate

Impacts of annealing temperature on microstructure, optical and electromagnetic properties of zinc ferrites nanoparticles synthesized by polymer assisted sol-gel method

Nanocrystalline zinc ferrite (NZF) were successfully synthesized at different calcination temperature via sol-gel method from the precursor salt solutions using tartaric acid and PVA solution as a chelating agent and binder respectively. The characterization of NZF and their properties had been investigated using sophisticated techniques viz. X-ray diffraction, Fourier transform infra-red spectroscopy, Scanning electron microscopy, Transmission electron microscopy, Energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, UV–Vis-NIR spectroscopy, Vibrating sample magnetometer and Impedance analyzer. X-ray peak profile analysis through Debye Scherer and Wilson method, Halder-Wagner method has been used to estimate the structural parameters. The crystallite size and particle size of ZnFe2O4 samples were found to increases with increasing annealing temperature while lattice parameters and lattice strain decreases. Dynamic light scattering and zeta potential measurements were used to evaluate the particle size distribution and stability of these systems. The room temperature magnetic properties measurement showed that the net magnetic moment is observed for NZF due to cation distribution although the bulk ZnFe2O4 is non-magnetic. Direct optical band gaps of the prepared NZF samples has been investigated by UV–Vis NIR spectroscopy using Tauc formula and found that energy band gaps (Eg) values are in a narrow range of 1.19–1.86 eV. The frequency dependent dielectric properties, impedance and modulus spectroscopy measurement has been investigated in the frequency range of 100 Hz to 20 MHz. The synthesized NZF particles will be applied for Gas sensor, humidity sensor and photocatalyst

Development of ceramic grade red iron oxide pigment from waste iron source

Ceramic grade red iron oxide (α-Fe2O3) nanoparticles pigments have been synthesized from waste condensed milk containers which contain a prominent amount of iron (93.2%). The synthesis method comprised of two steps: in the first step ferrous sulfate was prepared following an acid leaching method; while the second step was oxidation and calcination of ferrous sulfate to produce desired α-Fe2O3 in nano form. The structure, functional groups, chemical state, morphology, particle size, surface area, elemental, thermal analysis and magnetic properties of the samples were investigated using XRD, FTIR, XPS, SEM, BET, EDS, TG-DT and VSM respectively. Pure hematite (α-Fe2O3) phase was confirmed by XRD and the average crystal sizes were in the range 34–126 nm have been performed by Debye-Scherer's formula, which are consistent with the results as achieved from SEM images. Agglomerated irregular spherical nanoparticles (45–149 nm) were found in SEM image. The surface chemistry and the chemical state (Fe3+) of the hematite nanoparticles was also confirmed by XPS. The mesoporous nature of the nanoparticles with high surface area were measured by BET and it has been revealed that the BET specific surface area (33.55 m2/g) was marginally higher than the commercial one. The magnetic nature of the nanoparticles was portrayed by VSM and the nanoparticles showed the ferromagnetic behavior. Moreover, particle size distributions and zeta potential values have been also measured by DLS

Extraction and characterization of highly pure alumina (α, γ, and θ) polymorphs from waste beverage cans: A viable waste management approach

The recycling and recovery of important materials from inexpensive feedstock has now become an intriguing area and vital from commercial and environmental viewpoints. In the present work, extraction of different single phases of alumina (α, γ, θ-Al2O3) having high purity (>99.5 %) from locally available waste beverage cans (∼95 % Al) through facile precipitation route calcined at distinct temperatures has been reported. The optimization of process technology was done by a variety of different synthesis parameters, and the production cost was estimated between 84.47-87.45 USD per kg of alumina powder. The as prepared alumina fine particles have been characterized using different sophisticated techniques viz. TG-DTA, WD-XRF, XRD, FT-IR, SEM, DLS-based particle size analysis (PSA) with zeta (ζ) potential measurement and UV–Visible Spectroscopy. X-ray diffractogram confirms the formation of γ-, θ-, and α-alumina at 500–700 °C, 900–1000 °C, and 1200 °C respectively and crystallite size, crystallinity, strain, dislocation density, and specific surface area were measured using major X-ray diffraction peaks which varies with temperature. The SEM studies showed that the as prepared alumina particles were agglomerated, irregular-shaped with particle size (0.23–0.38 µm), pore size, and porosity were calculated from SEM image. ζ-potentials at different pH values as well as isoelectric point (IEP) of α, γ, and θ alumina were calculated in an aqueous medium which changes with temperature. The direct band gap (Eg) energies were found between 4.09 and 5.19 eV of alumina obtained from different calcination temperatures. The synthesized materials can be used in sensors, ceramics, catalysis, and insulation applications

Assessment of Reproductive Health Status and Quality of Life of Female Adolescents Living in the Slums of Dhaka, Bangladesh During COVID-19 Pandemic Situation: A Mixed-Method Study

Background: The COVID-19 pandemic has exacerbated the challenges of vulnerable adolescents who had reproductive health problems even before the COVID-19 pandemic. Methodology: We investigated this vulnerability through cross-sectional studies with a mixed-method approach. on female adolescents aged 15-19 years, residing in the Bauniabadh and the Ta block Jhil Par slums together with service providers. The quantitative method included a household survey of adolescents (n=144) through a semi-structured pre-tested questionnaire. The qualitative method included interviews with service providers (n=10) and with adolescents (n=9). Result: The study revealed changes in length, duration and flow of menstruation, substandard menstrual hygiene practices and impediments to the uptake of reproductive health (RH) information by adolescents during the pandemic. Married pregnant adolescents are inclined in taking their antenatal checkups (ANC) only during the last trimester and preferred delivery at home during the pandemic. There was also an increase in marriage among these adolescents and service providers had difficulty providing door-to-door RH services. Most of our female adolescents were married off during the pandemic, they lost connection with their friends and this made them feel lonely and secluded. They did not receive the support of their friends as before the pandemic. Conclusion: The study will enable the adolescent health expert to focus on the sexual and reproductive health (SRH) of vulnerable adolescents living in impoverished conditions during the COVID-19 pandemic

Exploration of properties (crystallographic, morphological, optical) of nano cobalt aluminate synthesized by facile sol–gel method: Effects of sintering temperature

The present work reports on the facile sol–gel synthesis of CoAl2O4 nanoparticles using cobalt nitrate and aluminum nitrate as the metal salts and citric acid and glycerol as chelating agents. The consequence of sintering temperature on the structure, particle size, morphology, composition, zeta potential, color, and reflectance spectra at neutral pH condition were explored with various instrumental techniques. The CoAl2O4 nanoparticles were characterized with Powder X-ray diffraction (PXRD), Fourier-transform infrared spectroscopy (FT-IR), Field emission scanning electron microscopy (FESEM), Energy dispersive spectroscopy (EDS), Nanoparticle size analyzer, Ultraviolet–Visible Diffuse Reflectance Spectroscopy (UV–Vis-DRS) and CIE-Lab colorimetric method. From the data of PXRD, the crystallite size and peak profile analysis were investigated by four different models. It was found that the average crystallite size varied in the range of 28.01–320.97 nm and single-phase cubic CoAl2O4 was formed without any impurity. The average particle size of CoAl2O4 nanoparticles was discerned from the FESEM images using ImageJ software and from a nanoparticle size analyzer. The average particle sizes were increased with the increasing sintering temperature. The values of zeta potential found in all of the samples represented high dispersion stability. From the colorimetry of CoAl2O4 nanoparticles, the CIE-La*b* output illustrated high purity and brightness and the spectra