Some aspects of the analytical chemistry of malathion

A thorough investigation of the recommended colorimetric method for the determination of malathion (an organophosphorus pesticide) has led to the identification of the major cause of all the problems with which the method suffers. The method, which involves the extraction of the copper (II) complex or the hydrolysis product of malathion from aqueous solution into immiscible organic solvents, has many drawbacks. For example, the colour of the organic extract fades very quickly and a slight increase in the contact time of the hydrolysis product and the copper reagent within the aqueous solution, results in a decrease in the ab-solute absorbance. Also, the presence of any reducing agents can be a significant source of error. In the present work, it has been shown that the basic cause of all these problems is the ability of copper (II) ion to be reduced to copper (I) ion. It has further been shown that these problems can be resolved by re-placing copper (II) by bismuth (III). This has led to the development of a modified colorimetric method for the determination. of malathion, which has distinct advantages over all other existing methods in terms of reagents required, ease in application, avoidance of interferences and stability of colour for extended periods of time. The modified colorimetric method described above has been further improved by making use of a ligand exchange reaction involving dithizone. The resulting final organic extract in this case is bright orange in colour, the absorbance of which can be measured even with simple photometers. The usefulness of the modified colorimetric method has been demonstrated by determining malathion in technical products, and in aqueous solution containing the compound down to sub ppm levels. The scope and applicability of atomic absorption spectrophotometry has been extended by demonstrating for the first time that the technique can be used for the indirect determination of malathion. Almost all of the work described above has been accepted for publication by international journals and considerable interest in the work has been shown by chemists working in the field of pesticide analysis and research

Development of a Method for the Determination of Chromium and Cadmium in Tannery Wastewater Using Laser-Induced Breakdown Spectroscopy

This paper illustrates systematic development of a convenient analytical method for the determination of chromium and cadmium in tannery wastewater using laser-induced breakdown spectroscopy (LIBS). A new approach was developed by which liquid was converted into solid phase sample surface using absorption paper for subsequent LIBS analysis. The optimized values of LIBS parameters were 146.7 mJ for chromium and 89.5 mJ for cadmium (laser pulse energy), 4.5 μs (delay time), 70 mm (lens to sample surface distance), and 7 mm (light collection system to sample surface distance). Optimized values of LIBS parameters demonstrated strong spectrum lines for each metal keeping the background noise at minimum level. The new method of preparing metal standards on absorption papers exhibited calibration curves with good linearity with correlation coefficients, R2 in the range of 0.992 to 0.998. The developed method was tested on real tannery wastewater samples for determination of chromium and cadmium

Comparing and Optimizing Nitrate Adsorption from Aqueous Solution Using Fe/Pt Bimetallic Nanoparticles and Anion Exchange Resins

This research work was carried out for the removal of nitrate from raw water for a drinking water supply. Nitrate is a widespread ground water contaminant. Methodology employed in this study included adsorption on metal based nanoparticles and ion exchange using anionic resins. Fe/Pt bimetallic nanoparticles were prepared in the laboratory, by the reduction of their respective salts using sodium borohydride. Scanning electron microscope, X-ray diffraction, energy dispersive spectrometry, and X-ray florescence techniques were utilized for characterization of bimetallic Fe/Pt nanoparticles. Optimum dose, pH, temperature, and contact time were determined for NO3- removal through batch tests, both for metal based nanoparticles and anionic exchange resin. Adsorption data fitted well the Langmuir isotherm and conformed to the pseudofirst-order kinetic model. Results indicated 97% reduction in nitrate by 0.25 mg/L of Fe/Pt nanoparticles at pH 7 and 83% reduction in nitrate was observed using 0.50 mg/L anionic exchange resins at pH 4 and contact time of one hour. Overall, Fe/Pt bimetallic nanoparticles demonstrated greater NO3- removal efficiency due to the small particle size, extremely large surface area (627 m2/g), and high adsorption capacity

The Normal Probability Distribution Function: An Alternate Derivation

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Removal of Fluoride from Drinking Water Using Modified Immobilized Activated Alumina

The study describes the removal of fluoride from drinking water using modified immobilized activated alumina (MIAA) prepared by sol-gel method. The modification was done by adding a specific amount of alum during the sol formation step. The fluoride removal efficiency of MIAA was 1.35 times higher as compared to normal immobilized activated alumina. A batch adsorption study was performed as a function of adsorbent dose, contact time, stirring rate, and initial fluoride concentration. More than 90% removal of fluoride was achieved within 60 minutes of contact time. The adsorption potential of MIAA was compared with activated charcoal which showed that the removal efficiency was about 10% more than the activated charcoal. Both the Langmuir and Freundlich adsorption isotherms fitted well for the fluoride adsorption on MIAA with the regression coefficient R2 of 0.99 and 0.98, respectively. MIAA can both be regenerated thermally and chemically. Adsorption experiments using MIAA were employed on real drinking water samples from a fluoride affected area. The study showed that modified immobilized activated alumina is an effective adsorbent for fluoride removal

Comparison of Adsorption Capability of Activated Carbon and Metal Doped TiO2 for Geosmin and 2-MIB Removal from Water

This study stemmed from consumer complaints about earthy and musty off-flavours in treated water of Rawal Lake Filtration Plant. In recent years, several novel adsorbents have been developed from nanomaterials for enhancing the contaminant removal efficiency. This paper presents preparation and the use of new adsorbents Pt doped titania and Fe doped titania, for the adsorption capacity of Geosmin and 2-MIB from water under laboratory conditions and their comparison, with most widely used activated carbon, under batch and column experiments. Stock solutions were prepared by using Geosmin and 2-MIB standards, procured by Sigma Aldrich (England). Samples were analysed using SPME-GC-FID. The adsorption of Geosmin and 2-MIB on GAC conformed to the Freundlich isotherm, while that of adsorption on metal doped titania fit equally well to both Langmuir and Freundlich isotherms. Moreover, data, generated for the kinetic isotherm, confirmed that Geosmin and 2-MIB removal is a function of contact time. Breakthrough column tests using 125 mg/L Pt doped titania nanoparticles, coated on glass beads against 700 ng/L of off-flavours, attained later breakthrough and exhaustion points and removed 98% of Geosmin and 97% of 2-MIB at room temperature. All columns could be regenerated using 50 mL 0.1 molar sodium hydroxide

Effect of Coating Thickness on the Properties of TiN Coatings Deposited on Tool Steels using Cathodic ARC PVD Techique

Titanium nitride (TiN) widely used as hard coating material, was coated on tool steels, namely on high-speed steel (HSS) and D2 tool steel by physical vapor deposition method. The study concentrated on cathodic arc physical vapor deposition (CAPVD), a technique used for the deposition of hard coatings for tooling applications, and which has many advantages. The main drawback of this technique, however, is the formation of macrodroplets (MDs) during deposition, resulting in films with rougher morphology. Various standard characterization techniques and equipment, such as electron microscopy, atomic force microscopy, hardness testing machine, scratch tester, and pin-on-disc machine, were used to analyze and quantify the following properties and parameters: surface morphology, thickness, hardness, adhesion, and coefficient of friction (COF) of the deposited coatings. Surface morphology revealed that the MDs produced during the etching stage, protruded through the TiN film, resulting in filmwith deteriorated surface features. Both coating thickness and indentation loads influenced the hardness of the deposited coatings. The coatings deposited on HSS exhibit better adhesion compared to those on D2 tool steel. Standard deviation indicates that the coating deposited with thickness around 6.7 μm showed the most stable trend of COF versus sliding distance

Photocatalytic Degradation of Nitro and Chlorophenols Using Doped and Undoped Titanium Dioxide Nanoparticles

Pure and Ag-TiO2 nanoparticles were synthesized, with the metallic doping being done using the Liquid Impregnation (LI) method. The resulting nanoparticles were characterized by analytical methods such as scanning electron micrographs (SEMs), Energy Dispersive Spectroscopy (EDS), and X-ray diffraction (XRD). XRD analysis indicated that the crystallite size of TiO2 was 27 nm to 42 nm while the crystallite size of Ag-TiO2 was 11.27 nm to 42.52 nm. The photocatalytic activity of pure TiO2 and silver doped TiO2 was tested by photocatalytic degradation of p-nitrophenol as a model compound. Ag-TiO2 nanoparticles exhibited better results (98% degradation) as compared to pure TiO2 nanoparticles (83% degradation) in 1 hour for the degradation of p-nitrophenol. Ag-TiO2 was further used for the photocatalytic degradation of 2,4-dichlorphenol (99% degradation), 2,5-dichlorophenol (98% degradation), and 2,4,6-trichlorophenol (96% degradation) in 1 hour. The degree of mineralization was tested by TOC experiment indicating that 2,4-DCP was completely mineralized, while 2,5-DCP was mineralized upto 95 percent and 2,4,6-TCP upto 86 percent within a period of 2 hours

EFFECT OF COATING THICKNESS ON THE PROPERTIES OF TiN COATINGS DEPOSITED ON TOOL STEELS USING CATHODIC ARC PVD TECHNIQUE

Titanium nitride (TiN) widely used as hard coating material, was coated on tool steels, namely on high-speed steel (HSS) and D2 tool steel by physical vapor deposition method. The study concentrated on cathodic arc physical vapor deposition (CAPVD), a technique used for the deposition of hard coatings for tooling applications, and which has many advantages. The main drawback of this technique, however, is the formation of macrodroplets (MDs) during deposition, resulting in films with rougher morphology. Various standard characterization techniques and equipment, such as electron microscopy, atomic force microscopy, hardness testing machine, scratch tester, and pin-on-disc machine, were used to analyze and quantify the following properties and parameters: surface morphology, thickness, hardness, adhesion, and coefficient of friction (COF) of the deposited coatings. Surface morphology revealed that the MDs produced during the etching stage, protruded through the TiN film, resulting in film with deteriorated surface features. Both coating thickness and indentation loads influenced the hardness of the deposited coatings. The coatings deposited on HSS exhibit better adhesion compared to those on D2 tool steel. Standard deviation indicates that the coating deposited with thickness around 6.7 μm showed the most stable trend of COF versus sliding distance.Morphology, surface roughness, coefficient of friction, hardness, adhesion