Extraction of acephate pesticide in environmental and agricultural samples by spectrophotometric method

In the present study, we have synthesis the azo dye for the reaction of p-amino antipyrine with HCl in NaNO₂ solution a 1:1 ​M ratio that was kept -5°C for 1–2 ​h, as result the absorption spectra observed at λ_max ​= ​460 ​nm. Beer’s law is obeyed over the awareness variety of 1 ​μg–100 ​μg ​mL^-1. The standard deviation and relative well-known deviation are 0.007 and 1.38%. The molar absorptivity and Sandell's sensitivity had been located to be 0.98 ​× ​10⁵ ​L ​mol^-1 ​cm^-1 and 0.99 ​× ​10^-3 ​μg ​cm^-2, respectively. Spectroscopy method used for the detection of Acephate pesticides on vegetable, fruit, soil, and water samples. FTIR method was used to consider and achieve structural information about the presented intermolecular interactions for vegetable samples. The eco-friendliness of the developed methods was assessed using the spectroscopy analytical tool on vegetables, fruit, soil, and water samples.     

Synthesis and characterization of reactive dyes based on 2-phenyl-3-[4′-(4″-aminophenylsulphonamido)]phenyl-4(3H)-quinazolinone-6-sulphonic acid

A series of new quinazolinone based mono azo reactive dyes (D_1–10) have been prepared by subsequent diazotization of 2-phenyl-3-[4′-(4″-aminophenylsulphonamido)]phenyl-4(3H)-quinazolinone-6-sulphonic acid (C) and coupling with various 4-chloro anilino cyanurated coupling components. These dyes give purple, red, orange and yellow color shades. All the reactive dyes were characterized by their percentage yield, UV–Vis spectroscopy, elemental analysis, IR spectroscopy, ¹H NMR spectroscopy and dyeing performance on silk, wool and cotton fibres. The percentage dye bath exhaustion on different fibres has been found to be reasonably good and acceptable. The dyed fibres show moderate to very good light fastness and good to excellent washing and rubbing fastness.     

Nano engineered biodegradable capsules for the encapsulation and kinetic release studies of ciprofloxacin hydrochloride

Polyelectrolyte based nano and micro capsules have been extensively studied as promising drug carrier in recent years. Natural degradable capsules have received great deal of attention due to their fascinating structural and morphological characteristics, biocompatibility, sustained and targeted-release capabilities. In this work, chitosan - dextran sulphate nano capsules were prepared via Layer-by-Layer (L-b-L) technique using sacrificial template for drug delivery applications. The loading and in vitro release studies were performed using ciprofloxacin hydrochloride as a model drug. The release media used in the study are plain water and Phosphate Buffered Saline (PBS). The optimum drug load was 389 ​μg, at a loading pH of 2.1 and a temperature of 25 ​°C for 50 ​min encapsulation time. The drug loaded capsules exhibited a slow and sustained release up to 24 ​h and the maximum release rate was obtained at pH 1.2 in water and pH 7.4 in PBS. Least amount of drug release occurred at pH 5.0 in both the release media. The amounts of drug release in water at pH 1.2, pH 5.0 and pH 7.4 are 309 ​μg, 163 ​μg and 251 ​μg respectively where as the corresponding values in the case of PBS (at pH 1.2, pH 5.0 and pH 7.4) are 236 ​μg, 198 ​μg and 251 ​μg respectively. Two different models namely, Ritger - Peppas and Higuchi models were chosen to study the release kinetics behaviour of ciprofloxacin hydrochloride. The prepared bio-degradable capsules had potential as drug carrier for targeting antibacterial drugs with diverse functionality.     

Dyeing behaviour of lyocell fabric: effect of NaOH pre-treatment

To understand the effect of alkali pre-treatment on the dyeing of lyocell fabrics, samples are pre-treated with 0.0–7.0 mol dm⁻³ NaOH using a pad-batch process and then dyed with different types of reactive dyes. Exhaustion, fixation, and visual colour strength (K/S values) are measured. It is observed that sodium hydroxide pre-treatment significantly improves the colour yield, exhaustion, and fixation for all dyes used. Highest K/S values are obtained when the fabrics are pre-treated with 2.0–2.5 mol dm⁻³ NaOH. Cross-sectional analysis shows that below this optimum concentration the core fibres in the yarn are not dyed; at optimum concentration all fibres in yarn cross-section are homogeneously dyed. Cross-sectional analysis shows that as the pre-treatment concentration of NaOH increases above 2.5 mol dm⁻³, the fibres change progressively from a circular to angular cross-section, forming a solid unit. The decrease in K/S above the treatment concentration of 2.5 mol dm⁻³, though the %E and %F remains almost constant, is attributed to the distribution of dye over a larger surface area of the outer fibres in the yarn cross section, forcing the K/S at λ_max to decrease. This paper was presented at the 2nd International Cellulose Conference, Tokyo, Japan, 24th October 2007.     

Preparation of highly selective solid-phase extractants for Cibacron reactive dyes using molecularly imprinted polymers

Selective polymeric extractants were prepared for preconcentration of Cibacron reactive red dye, a dye that is often applied with Cibacron reactive blue and Cibacron reactive yellow for dyeing of fabrics. The best extractant was fabricated (in chloroform) using methacrylic acid (as monomer), ethylene glycol dimethacrylate (as crosslinker), AIBN (as initiator for polymerization), and red dye as template molecule, with a molar stoichiometric ratio of 8.0:40.0:2.5:0.63, respectively. The structure of the molecularly imprinted polymer (MIP) was robust, and resisted dissolution up to 260 °C. Compared with the un-imprinted polymer, the imprinted product has a large specific surface area which improved its adsorption capacity. The effect of imprinting was obvious from the adsorption capacity measured at pH 4 for red dye (the imprinted molecule), which was increased from 24.0 to 79.3 mg g⁻¹ after imprinting. Equilibrium adsorption studies revealed that the dye-imprinted-polymer enables efficient extraction of red dye even in the presence of blue and yellow dyes which have similar chemical natures to the red dye. The selectivity coefficients S _{red dye/dye}, were 13.9 and 17.1 relative to the yellow and blue dyes, respectively. The MIP was found to be effective for red dye preconcentration, with a preconcentration factor of 100, from tap water and treated textile wastewater. The factors affecting extraction of red dye by the MIP were studied and optimized. Under the optimized extraction conditions, red dye was selectively quantified in the presence of other competing dyes at a concentration of 20 μg L⁻¹ from different water systems with satisfactory recoveries (91–95%) and RSD values (∼5.0%).     

CI Reactive Black 5 dye as a visible crosslinker to improve physical properties of lyocell fabrics

Bi-functional reactive dyes have been used for reducing the fibrillation of lyocell fibres. The sole influence of CI Reactive Black 5 dye on the fibrillation tendency of lyocell single jersey knitted fabrics was investigated by dyeing with different concentrations (35 g/L for medium shade and 70 g/L for dark shade), dyeing without dyestuff and by decolouration process after each dyeing. The fibrillation tendency of lyocell fibres was accessed by means of fibre wet abrasion resistance and fibrillation number. Nitrogen content was used as indication of the amount of reactive dye in fabrics during dyeing and decolouration processes. The correlation between fibre fibrillation tendency and colour values of fabrics was found. Due to the fibrillation reduction, pilling formation in dyed lyocell fabrics was improved. As colour values can estimate the dye fixation and reduction in fabrics, reactive dye can be used as a visible marker for crosslinking effect on lyocell fabrics.     

Photo-catalytic degradation of different toxic dyes using silver nanoparticles as photo-catalyst,mediated via Citrus aurantium peels extract

Green synthesis of silver nanoparticles was accomplished using peels (rind) extract of Citrus aurantium as a reducing as well as capping agent. Biosynthesized AgNPs (silver nanoparticle) has been characterized via UV–Visible spectroscopy, XRD, SEM, EDAX, TEM and TGA. The observed UV–Vis analysis resulted in the formation of characteristic surface plasmon resonance absorption band centered at 465 ​nm. The observed XRD patterns, having hkl values (111), (200), (220) and (222), confirms the cubic crystalline structure of AgNPs. The average grain size 9.5 ​μm was observed by the SEM technique. Bio synthesized AgNPs were efficiently degrading the methylene blue dye nearly 95.35% in 98 ​h of exposure time. It also degraded acridine orange dye 87.34% and rose bengal dye 90.09% followed by 4h of continuous UV absorption. It also degrades methyl orange dye nearly 51% in 10h of solar irradiation. Synthesized AgNPs can be used as photo-catalyst for degrading toxic dyes.     

Zeolite Y from kaolin clay of Kachchh,India: Synthesis,characterization and catalytic application

Kaolin clay obtained from Kachchh, Gujarat was used as alumina and silica source to synthesize zeolite Y by hydrothermal method. The synthesis route comprised of the following steps: sulfuric acid treatment at 110 ​°C (4 ​h) for impurity removal followed by calcination at 600 ​°C for 4 ​h, thermal activation of kaolin into metakaolin by NaOH fusion at 850 ​°C (8 ​h); aging of reaction mixtures at 50 ​°C (24 ​h); crystallization (24 ​h) followed by washing and drying. The synthesized zeolite Y was examined by multiple characterization techniques which revealed a pore volume of 0.22 ​cm³/g with pore size of 2.89 ​nm having essential surface area of 320 ​m²/g, indicating a porous material having majority of micropores and remaining mesopores. The zeolite exhibited good catalytic activity for succinic acid esterification using ethanol to produce monoethyl and diethyl succinate. The conversion of SA (72%) and yield (60%) of valuable diester indicated good conversion rate and selectivity at moderate reaction conditions. Detailed structural comparison with zeolite Y synthesized using standard chemical route is also carried out. This work demonstrated an effective way of preparing environmentally benign porous zeolite Y having high surface area and pore volume that can be useful for catalytic applications.     

Screening,isolation and selection of a potent lipase producing microorganism and its use in the kinetic resolution of drug intermediates

Lipases are ubiquitous enzymes that belong to family of serine hydolases with a wide variety of industrial applications. This study reports isolation, screening and identification of enantioselctive lipase producing microorganism for kinetic resolution of racemic alcohols. For this, we collected soil samples from different oil rich environments and we performed primary screening that was by carried out by using MSM-tributryin clear zone assay. The selected samples from first screen were subjected to secondary screening to distinguish lipase producing strains from esterase producing strains using p-nitrophenyl palmitate lipase assay. In tertiary screening, 16 lipase producing strains that were identified in secondary screening were employed for resolution of 5 different (RS)-alcohols. Out of all 16 lipase producing strains, only one strain selectively converted 3 racemic alcohols. Based on morphological, biochemical and physiological characteristics, and 16S rRNA gene sequencing, the strain was identified as Pseudomonas beteli. The strain was found to be S-selective and there been no reports on use of Pseudomonas beteli lipase for kinetic resolution of alcohols. The lipase activity was further increased by media optimization and by improving growth conditions, and production of lipase in shake flask study as well as in laboratory scale fermenter. The optimum time for enzyme production by Pseudomonas beteli was 96 ​h whereas cell mass growth was highest at 72 ​h. Optimum temperature and pH were 30 ​°C and 6, respectively. Beef extract (5 ​g/L), peptone (5 ​g/L), sodium chloride (5 ​g/L), yeast extract (1 ​g/L) and glucose (5 ​g/L) were found as optimum nutrition sources for the cell mass growth and lipase production by Pseudomonas sp. Overall, 3.4 times higher enzyme activity and 2.75 times higher cell mass growth were achieved in bioreactor in comparison to the shake flask study. Lipase having high titer was employed successfully for the kinetic resolution of several drug intermediates.     

Photophysical insights on quantum dots-zinc porphyrazine system studied in solution

The present study reports spontaneous interaction of a quantum dots, namely, CdS_xSe_1-x/ZnS (QD) with zinc porphyrazine (1) in toluene. It is observed from steady state fluorescence measurements that photoluminescence of QD suffers quenching by 1. Time resolved fluorescence measurements reveal small change in the lifetime of QD (16.10 ns) following it interaction with 1 (15.77 ns). The magnitude of k_q for QD-1 system, i.e., k_q ​= ​5.25 ​× ​10¹² ​L⋅mol⁻¹⋅sec⁻¹ (evaluated from the stern-volmer plot) establishes that photoexcited QD undergoes decay by 1 according to static quenching mechanism. The results emerging from above study confirm that QD-1 system may be judiciously applied as an energy storage material in near future.     

Synthesis and fluorescence characteristics of novel asymmetric cyanine dyes for DNA detection

Sixteen new asymmetric monomethine cyanine dyes have been synthesized and their spectral characteristics and interaction with double stranded DNA have been investigated. The dyes absorb in the region 453–519 nm and have molar absorptivities in the range 37.900–93.100 l M^?1 cm^?1. The dyes do not have intrinsic fluorescence, but in the presence of dsDNA they exhibited a significant enhancement in fluorescence. The most pronounced increase was found for D9, D10, D12 and D16 allowing the recommendation of these dyes as the most sensitive DNA markers. Thermodynamic analysis of cyanine–DNA complexation was carried out using the McGhee & von Hippel non-cooperative excluded site model, and binding parameters have been derived. A hypothesis describing the DNA–dye binding mode has been proposed.     

Coordination of reduced Schiff base anion to Pd(II): Synthesis,characterization, DFT calculation and catecholase activity

The article reports the synthesis and characterization of a new palladium(II) complex of type [(L_NNN¹⁻)PdCl] (1) where L_NNN¹⁻ is a mono anionic Schiff's base having a imine bond in reduced state. The L_NNN¹⁻ is generated from a tridentate NNN donor ligand (L_NNN) through in-situ reduction using sodium borohydride, where L_NNN is [(E)-N-(phenyl(pyridine-2-yl)methylene)quinoline-8-amine)]. 1 is characterized by the single crystal X-ray diffraction study, IR, mass and UV–Vis spectroscopy. The X-ray bond parameter authenticates the imine bond of the coordinated Schiff's base anion is in reduced state. 1 exhibits catalytic activity towards the oxidation of 3,5-ditertiarybutyl catechol(3,5-DTBC) with turnover number (K_cat) ​= ​135.6 h^-1. The catalytic oxidation of 3,5-DTBC is authenticated by the UV–Vis, mass and EPR spectroscopy. An isotropic EPR signal with g ​= ​2.011 of a solution containing 1 and 3,5-DTBC authenticating the generation of organic radical during the oxidation process. Cyclic voltammogram of 1 displays an irreversible anodic wave at +0.22 ​V may be due to the oxidation of N⁻ to N^•−. The atomic spin density of 1⁺ obtained from DFT calculation is also supporting the N-centre oxidation process.     

Synthesis and application of disazo reactive dyes derived from sulfatoethylsulfone pyrazolo[1,5-a]pyrimidine derivatives

Two models of heterocyclic reactive dyes based on disazo pyrazoloprymidine derivatives and possessing a sulfatoethylsulfone reactive group were synthesized and characterized by elemental analysis, IR and ¹H NMR spectroscopy. The dyes were applied to cotton, wool and silk fabrics. Effects of varying dyeing conditions were investigated. The results assessed for the exhaust dyeing methods on the different fabrics indicate that these reactive dyes showed high exhaustion and fixation values. The dyed fabrics also showed very good light fastness and good to excellent washing, rubbing and perspiration fastness.     

Application of Artificial Neural Network and Particle Swarm Optimization for modelling and optimization of biosorption of Lead(II) and Nickel(II) from wastewater using dead cyanobacterial biomass

Removal of heavy metals through biosorption using biomass offers several advantages over other conventional techniques such as low cost, high efficiency, environmentally friendly, etc. In the present article, biosorption of Nickel(II) and Lead(II)was investigated using dried biomass of cyanobacterial consortium. OFAT (one-factor-at-a-time) analysis was used to assess the effect of input parameters on the removal of potentially toxic elements by varying initial metal ion concentration (2–10 mgL⁻¹), adsorbent dose (0.1–1.0 gL^-1), pH (for Pb(II): 2–6, for Ni(II): 2–8) and temperature (25°C–45°C) individually, at constant shaking speed of 150 ​rpm. Results showed that removal using biomass attained highest values in as short time as 15 ​min. The investigations also showed the removal is highly effective at lower initial concentrations of heavy metals. Maximum removal of Lead(II) (87.27 ​± ​1.75%) and Nickel(II) (92.57 ​± ​0.77%) was obtained at pH 6 and 45°C and at pH 7 and 25°C, respectively, within 15 ​min with 0.1 gL^-1 biomass. Both the Langmuir model and Freundlich model were seen to fit the equilibrium data. Further, Artificial Neural Network was used to model the biosorption process. Subsequently, Particle Swarm Optimization was applied to optimize the operating conditions for the removal of both the metals.     

Effect on rheology and frying stability of edible oil before and after addition of fenugreek seeds

Rheological parameters of vegetable oils showed great changes during frying. The correlation between rheological behavior and viscosity measurements during frying can give a good overall estimate of frying oil quality. In the present study, rheological properties of rice bran oil (RBO) and soybean oil (SBO) during deep-frying of 13 ​min were investigated for consecutive 1st, 2nd, 3rd, and 4th frying at an interval of one week. To enhance the frying stability of RBO and SBO, fenugreek seeds (Trigonellafoenum graecum) was added during frying. The shear stress versus shear rate data was fitted to Newtonian and Herschel-Bulkley rheological models. The flow behavior of RBO and SBO with and without fenugreek seeds in before and after frying were measured at 30 ​± ​2 ​°C. The increase in viscosity, acid values and flow behavior index (n) with frying times for both RBO and SBO can be controlled with the addition of fenugreek seed up to 3rd frying with n ​< ​1 values, where without fenugreek seeds for RBO and SBO it showed a shear thickening properties (n ​> ​1) after 2nd and 3rd frying respectively.     

Application of newly synthesized bisazo dichloro-s-triazinyl reactive dyes bearing 1,3,4-oxadiazole molecule

Novel bisazo dichloro-s-triazinyl (DCT) reactive dyes (5a–h) containing 1,3,4-oxadiazole molecule as a tetrazo component were synthesized and applied on silk, wool and cotton fibers by exhaust dyeing method. The structures of these dyes were confirmed by UV–vis, FT-IR, ¹H and ¹³C NMR and elemental analyses. The exhaustion, fixation and fastness properties of the dyed fabric were assessed and the results demonstrated that these dyes showed moderate to very good light and good to excellent washing and rubbing fastness properties. The colorimetric data (L¹, a¹, b¹, C¹, H¹, K/S) of these dyes have also been studied in detail.     

Hydrolyse und Alkoholyse von Reaktivfarbstoffen: II. Hydrolyse von Monochlortriazin-Farbstoffen. 2. Mitteilung über reaktionsmechanistische Untersuchungen an Reaktivfarbstoffen

• 1 The kinetics of the hydrolysis of three monochlorotriazine reactive dyes have been determined in alkaline buffer solutions at 60°, 80° and 98° (ionic strength I = 0.0625).
• 2 The kinetic results as well as diffusion measurements in aqueous solution indicated that these dyes form aggregates at dye concentrations at 6 · 10^?4, but practically not at 6·10^?6 moles/l.
• 3 The reaction order with respect to hydroxyl ions has been determined. The influence of general base concentration was negligible.

     

Synthesis and characterization of penta-coordinated copper(II) complexes with hydrazido based ligand and imidazole as auxiliary ligand

The reaction of (Z)-2-(phenyl(2-(pyridin-2-yl)hydrazono)methyl)pyridine (L) and copper(II) salt in methanol yields a series of five pentacoordinated mononuclear complexes. The molecular formulations of these complexes are as [Cu(L)(ImH)₂](ClO₄)₂ (1), [Cu(L)(2-MeImH)₂](ClO₄)₂ (2), [Cu(L)(2-EthImH)₂](ClO₄)₂ (3), [Cu(L)(BenzImH)₂](ClO₄)₂ (4) and [Cu(L)(2-MeBenzImH)₂](ClO₄)₂ (5) (where ImH ​= ​Imidazole, 2-MeImH ​= ​2-Methylimidazole, 2-EthImH ​= ​2-Ethylimidazole, BenzImH ​= ​Benzimidazole, 2-MeBenzImH ​= ​2-Methylbenzimidazole). The room temperature magnetic moment values are in the range 1.79–1.81 B ​M. The conductance measurements suggest that they are electrolytic in nature. The DFT calculations were performed to get information about the structures of the complexes. The copper(II) centre in all complexes is a Penta-coordinated. The proligand has NNN donor sites viz., two pyridine N and one azomethine N atoms, whereas co-ligand coordinates through pyridine N atom forming two five-membered chelate rings. The τ₅ values of these complexes are in the range 0.177–0.495. Both pro and co-ligands are neutral. X-band Epr spectral measurements have been carried out to authenticate the paramagnetic behaviours of all complexes. The stability of the copper(II) centre was examined using cyclic and differential pulse Voltammetry. The IC₅₀ and SOD activity values for all complexes reveal that they are good SOD active complexes. The IC₅₀ value of present complexes remains in the range 26–43 ​μM.     

Sorption of dyes on cellulose II: effect of alkali treatment of fibre and dye structure

Cellulose is a linear 1,4-β-glucan polymer where the units are able to form highly ordered structures, as a result of extensive interaction through intra- and intermolecular hydrogen bonding of the three hydroxyl groups in each cellulose unit. Alkali has a substantial influence on morphological, molecular and supramolecular properties of cellulose II polymer fibres causing changes in crystallinity. Lyocell fibres pre-treated with 0.0, 2.0, and 4.0 mol dm⁻³ aqueous NaOH solution were dyed with hydrolyzed reactive dyes that had different molecular shapes and sizes. Overall exhaustion (q _e), value of K, and −ΔG increased for lyocell samples pre-treated with aqueous NaOH solution in the following order: 2.0 > 4.0 > 0.0 mol dm⁻³ NaOH. The same trends were observed for colour strength (K/S) values of the dyeings. Pre-treatment of lyocell with 2.0 mol dm⁻³ NaOH creates the substrate that achieves the most thermodynamically favourable system for sorption of hydrolyzed reactive dyes, as at this concentration crystallinity decreases (with respect to 0.0 mol dm⁻³ NaOH treated lyocell) to afford higher sorption; however, at higher alkali concentrations the macro-sorbent forms a compacted unit that limits diffusion within the sorbent interior. Molecular size of the sorbate dye has a significant effect on the sorption process: for the largest dye structure the sorption isotherm is most closely correlated to a Langmuir isotherm; as the size of the dye decreases correlation to a Langmuir isotherm is observed, but with good correlation to the Freundlich isotherm; as the size of the dye is decreased further sorption is more typical of a Freundlich isotherm.     

Experiment of subcritical water (Fenton) oxidation treatment of methyl vanillin wastewater

In this paper the oxidative degradation process of methyl vanillin wastewater was studied by the subcritical water oxidation (HCWO) technology. A subcritical Fenton oxidation (HCFO) system formed while Fe²⁺ was added as a catalyst. The oxidation degradation kinetics of methyl vanillin wastewater was also studied. The results showed that the suitable process conditions for degradation of methyl vanillin wastewater by HCWO were as follows: temperature of 340 ​°C, pressure of 24 ​MPa, oxidant multiple of 1.5, residence time of 217.3 ​s (flow rate of 2.0 ​mL ​min^-1). For methyl vanillin wastewater, the HCFO system has no obvious advantages compared to the HCWO system. The activation energy (Ea) of HCWO oxidized methyl vanillin wastewater reaction was 32.6 ​kJ ​mol^-1, and the pre-exponential factor A was 5.64 s^-1.