Mercuric Acetate Research Articles

Development of non-aqueous titrimetric and spectrophotometric methods for the determination of valganciclovir hydrochloride in bulk drug and tablets

Two non-aqueous titrimetric and one visible spectrophotometric methods were developed and validated for the determination of valganciclovir hydrochloride (VLGH) in pure drug and tablets. The titrimetric methods were carried out by titrating the VLGH solution in glacial acetic acid with acetous perchloric acid (HClO4) in the presence of mercuric acetate and the end point of this titration was being located either visually (method A) or potentiometrically (method B). The spectrophotometric method (method C) was based on the addition of p-dimethylaminobenzaldehyde (DMAB) solution to VLGH solution and the formed yellow condensation product was measured at 420nm. In titrimetric procedures, both the methods A and B were applicable over the range of 4-20mg VLGH, and the calculations were based on a 1:1 reaction stoichiometry (VLGH:HClO4). In a spectrophotometric method, Beer's law was valid in a concentration range of 5-50 μg/mL VLGH with the corresponding value of molar absorptivity of 4.43×103L/mol cm for method C. The limits of detection (LOD) and quantification (LOQ) for method C were 0.3 and 0.92μg/mL, respectively. The developed methods were successfully applied to the determination of VLGH in tablets, and the results were statistically compared with those of a reference method by applying Student's t-test and F-test. Further, the validity of the developed methods was confirmed by recovery studies via standard addition technique.

Electrochemical sensor studies and optical analysis of developed clay based CoFe2O4 ferrite NPs

The Cobalt ferrite (CoFe2O4) and Clay/CoFe2O4 has been successfully synthesized via chemical method have been investigated. The structural properties of the produced powders were investigated using X-ray diffraction (XRD) and Field emission scanning electron microscopy (FE-SEM). XRD patterns confirms the spinel/cubic structure of the prepared Clay/CoFe2O4. FE-SEM micrographs showed uniform sphere-shaped CoFe2O4 when infused with the clay. In addition, Infrared spectroscopy has been used to verify cobalt ferrite formation and Clay/CoFe2O4 particles. The photocatalytic performance of Clay/CoFe2O4 was examined for their potential role in photo degradation of Indigo carmine dye under UV-light. The result shows that the composite is suitable for excellent photocatalytic degradation performance and degradation was found to be 98 %. Electrochemical analysis was conducted for the synthesized material with prepared Nickel mesh electrode in 0.1 M KOH electrolyte. It showed excellent performance in redox potential measured by cyclic voltammetry and extended their sensor activities towards chemical sensors (arsenic trioxide, lead acetate, mercuric acetate and stannous chloride). These studies showed new platform to use simple chemical method for the preparation of Clay/CoFe2O4 for their potential applications such as in detection of heavy metals, waste water treatment and electrochemical studies.

Synthesis and characterization of novel Hg(II) complexes with new Schiff bases

The research included the use of new Schiff's bases to prepare novel mercury (II) complexes as follows:Schiff's bases ligands prepared using aromatic aldehydes and various aromatic primary amines [S1-S6]. Six mercury complexes [H1-H6] were prepared by the interaction of mild moles of organic Schiff's bases with 1 mol of mercury salt (CH3COO)2Hg. The Schiff's bases prepared spectroscopes were diagnosed by the UV–visible spectrum, the infrared spectrum (FT-IR), and the nuclear magnetic resonance spectrum (1H NMR). The reaction mechanism was proposed in light of these results, as it confirmed the validity of the proposed chemical compositions. Metallic complexes prepared spectrally were diagnosed by the UV–visible spectrum, the infrared spectrum and the mass spectrum (Lc-Mass), and analysis of the elements C.H.N.S. The mechanism of interaction was suggested in light of these results, as it confirmed the validity of the proposed chemical compositions, magnetic and electrical conductivity sensitivity of all the prepared complexes was measured. Lc-Mass spectrum results, analysis of the elements C.H.N.S, measurement of molar conductivity, magnetic moment measurements have proven that azomethine compounds interacting with cadmium chloride and mercury acetate are di ligand.

Mechanistic and thermodynamic aspects of oxidative removal of flucloxacillin by different oxidants in an acidic medium

The mechanism of oxidative removal of flucloxacillin antibiotic (Flx) by two different oxidants (Ox), potassium bromate (KBrO3) and potassium iodate (KIO3), were studied using a spectrophotometric technique in sulfuric acid medium. The stoichiometry of the oxidation reactions of flucloxacillin by both oxidants was set to be a 2: 3 (Ox: Flx). The oxidation products of flucloxacillin were identified utilizing spot tests and FT-IR spectroscopy. The reactions followed a first order credence in [Flx] and lesser than unit order kinetics regarding to both [Ox] and [H+]. Negligible impacts of both ionic strength and dielectric constant of the reactions medium on the rates of reactions were observed. The dependence of the oxidation rates on mercuric acetate concentration which works as a scavenger for any bromide or iodide ion composed during the reactions was investigated. Credence of reaction rates on temperature was studied, and the activation parameters were assessed and discussed. Tests for free radicals involvement throughout the oxidation reactions were negative. The reactions mechanism was elucidated and the rate law expressions were derived.

Features of the Reaction of Dimedone with Some Amines in the Presence of Mercury(II) Acetate

Regiochemistry of the reaction of N-substituted propargylamines with dimedone in the presence of mercury(II) acetate was studied. Xanthene and diene derivatives, as well as symmetric mercury aminopropinides, were obtained, for one of which the crystallographic parameters are given.

Kinetics and mechanism of oxidation of creatine by N-Bromosuccinimide in acidic aqueous medium

The kinetics and the mechanism of oxidation of creatine (AA) by N-Bromosuccinimide (NBS) in an acidic aqueous medium were examined under isolation conditions. Iodometric method was used to follow the unconsumed NBS at different time intervals. Mercuric(II) acetate was used as a scavenger to capture any Br- formed during the reaction and hence to avoid autocatalytic oxidation by bromine. Findings from stoichiometry measurements revealed that the reaction between AA and NBS was a 2:1 molar ratio. The kinetic study showed that the reaction was first order with respect to both AA and NBS. Increasing [H+] had a negative effect on the rate of reaction. The effect that varying the solvent composition has on the rate of reaction was investigated, and it was found that the reaction rate decreased as the dielectric constant of the solvent increased. The temperature dependence was determined under fixed experimental conditions, from which thermodynamic parameters were calculated. From the proposed mechanism, a rate law was established that was in strong agreement with experimental kinetics.

The Reaction of (1,3,4-Oxadiazole-Thiolato) Mercury(II) with Triphenyl Phosphine

The reaction of 5-phenyl-1,3,4-oxadiazole-2-thiol with mercury(II) acetate in ethanol led to the isolation of the complex [Hg(L)2] (1). Further reaction of 1 with a twofold molar excess of triphenylphosphine led to the isolation of [Hg(L)2(PPh3)2] (2). The complex 2 was characterized by infrared, ultraviolet–visible and nuclear magnetic resonance spectroscopy techniques, as well as by X-ray diffraction analysis.

Measurement Device for Ambient Carbonyl Sulfide by Means of Catalytic Reduction Followed by Wet Scrubbing/Fluorescence Detection.

A portable chemical analysis system for monitoring ambient carbonyl sulfide (COS) was investigated for the first time. COS is paid attention to from the perspectives of photosynthesis tracer, breath diagnosis marker, and new process-use in the manufacture of semiconductors. Recently, the threshold level value of COS was settled at 5 ppm in volume ratio (ppmv) for workplace safety management. In this work, COS was converted to H2S by a small column packed with alumina catalyzer at 65 °C. Then, the H2S produced was collected in a small channel scrubber to react with fluorescein mercuric acetate (FMA), and the resulting fluorescence quenching was monitored using an LED/photodiode-based miniature detector. The miniature channel scrubber was re-examined to determine its robustness and easy fabrication, and conditions of the catalyzer were optimized. When the FMA concentration used was 1 μM, the limit of detection and dynamic range, which were both proportional to the FMA concentration, were 0.07 and 25 ppbv, respectively. Ambient COS in the background level and even contaminated COS in the nitrogen gas cylinder could be detected. If necessary, H2S was removed selectively by reproducible adsorbent columns. COS concentrations of engine exhaust were measured by the proposed method and by cryo-trap-gas chromatography-flame photometric detection, and the results obtained (0.5–5.9 ppbv) by the two methods agreed well (R2 = 0.945, n = 19). COS in ambient air and exhaust gases was successfully measured without any batchwise pretreatment.

Evaluation of Analytical Results Obtained From Standard AOAC Method and Accelerated Wijs Method for the Determination of Iodine Value of Different Brands of Mustard Edible Oils

In the present work, accelerated method is used for the measurement of iodine value, wherein mercuric acetate is directly used in the powder form. The method only requires to add the catalyst mercuric acetate in the process of determination without changing the operational steps of the Wijs method. Compared with the Wijs method in which it will take at least 30 minutes to finish it, the rapid determination method can make the determination reaction finished in 3 minutes. The iodine value of different vegetable oils such as Kacchighani mustard oil (Kgmu, Dalda),Kacchighani mustard oil (Kgmu1,Mahakosh), Kacchighani mustard oil (Kgmu2,Tez),premium mustard oil kacchighaani (Pmukg, RRO Mustdil), Kacchighani mustard oil (Kgmu3,Nature fresh) and Kacchighani mustard oil (Kgmu4, Engine)oils were determined by regular Wijs method for 30 minutes whereas when we apply catalytic Wijs method with use of 2 mg, 5 mg and 10 mg of mercuric acetate to perform as catalyst then it is reducing the time of analysis to 3 minutes. When catalyst is used the different values obtained for standard deviations are 0.14 for 2mg, 0.27for 5mg and 0.3 for 10 mg whereas 0.35 for non catalyst addition. The results obtained in this present work aremore % difference in IV of pure kacchighani mustard oil (Pkgmu)and Kacchighani mustard oil (Kgmu2).

3D-printed and fully portable fluorescent-based platform for sulfide determination in waters combining vapor generation extraction and digital images treatment

The determination of sulfide anion in a variety of waters (e.g. wastewaters and natural waters) even at low concentration (i.e. in the μM range) is essential due to its high toxicity, corrosivity and unpleasant smelling proprieties. Despite several methodologies are dedicated to aqueous sulfide determination, most of them need sampling/transport steps – which is no adequate to sulfide due to its reactivity and instability – resulting in critical analytical bias. In this study, we present a fully modular and portable 3D-printed platform for in-situ aqueous sulfide determination. The analytical device is based on H2S vapor generation from the sulfide sample solution by addition of H3PO4 followed by collection in a miniaturized cuvette (μCuvette) containing few microliters of Fluorescein Mercury Acetate (FMA), a fluorescent dye. The chemical reaction results in fluorescence quenching of the dye at 530 nm when excited at 470 nm. A light-emitted diode (LED) emitting at 470 nm and powered with 9 V-battery based circuitry was employed to provide stable excitation light source at 20 mA. Digital images from the light emitted by FMA were captured by a smartphone and the Green channel intensity was used as analytical signal. Under optimized conditions, a linear relation (r2 > 0.99) from 0.1 to 5 μM of sulfide was obtained using 10 mL of standard/sample solution. The portable platform was applied to the in-situ monitoring of sulfide in tap water and river water with no loss of analyte, no need for external power supplies or powered pumps. and the analysis results were obtained in 20 min. The proposed device shows advantages in terms of high degree of portability, low-power consumption, easiness to use, minimal use of reagents yet enabling on-site determination of sulfide with high sensitivity. By using the vapor generation approach combined with the modular building blocks concept presented herein for the first time, we anticipate the development of a tailored “plug-and-play” platform enabling the multiplexed determination of volatile substances using absorbance, reflectance or fluorescence measurements with smartphones.

Synthesis, characterization and H2 uptake of novel Hg(II) complexes containing 1,4-benzothiazin-3-one

Abstract Treatment of 1,4-benzothiazin-3-one (Hbto) with mercury(II) acetate Hg(OAc)2 in 2:1 mol ratio affords [Hg(bto)2] (1) in 99% yield. The resulted complex was used as a synthon to prepare new mixed-ligand complexes with monophosphines or diphosphines of the types [Hg(bto)2(L)2] or [Hg(bto)2(L-L)]; where L = triphenylphosphine (Ph3P) (2) or triphenylphosphinesulfide (Ph3PS) (3); L-L = 1,2-bis(diphenylphosphino)ethane (dppe) (4) or 1,1′-bis(diphenylphosphine)ferrocene (dppf) (5). FTIR, 1H NMR, 13C NMR, 31P-{1H} NMR, molar conductivity and elemental analysis were used to characterize the resulted complexes. Results suggest that 'bto' ion in [Hg(bto)2] (1) is linked to mercury ion via exocyclic oxygen and endocyclic nitrogen atoms in a chelating bidentate fashion while in the complexes (2–5), it is linked to mercury ion via endocyclic nitrogen atom in a monodentate fashion. Furthermore, to take benefit of mercury complexes which were classified as toxic compounds, [Hg(bto)2] (1) complex has been evaluated for its susceptibility to hydrogen storage. The result of H2 storage showed that this complex can store 1.42 wt% of hydrogen under 88 bar and 77 K.

In-situ approach for the synthesis of bromide-bridged mercury(II) N-heterocyclic carbene complexes

The study was designed to synthesize bromide-bridged mercury(II) symmetric and non-symmetric N-heterocyclic carbene complexes. The preparation of benzimidazolium salts (4–6) was accomplished by symmetrical and non-symmetrical substitution on benzimidazole. The salts were subjected to an in-situ process for metallation to get [Hg(II)-NHC] complexes [(HgBr-NHC)(µ2Br)2] (7–9) by reacting benzimidazolium salts (4–6) with mercury(II) acetate at room temperature. Compounds were characterized by elemental analyses, FT-IR and NMR spectroscopy. Single crystals of 7 and 8 were analyzed by X-ray crystallographic technique which showed tetrahedral dinuclear complexes with two bridging bromides. An attempt to explore the feasibility of redox transmetallation approach (RTM) for synthesis of ytterbium complexes was also carried out by reacting 7–9 with ytterbium powder under inert atmosphere. The products were metallic mercury, benzimidazolium salts, and ytterbium bromide instead of ytterbium complexes.

Mercuration and Telluration of 2-Fluoro-5-nitroaniline: Synthesis, Antibacterial, and Computational Study

New derivatives of organotellurium and organomercury compounds have been synthesized in the reaction of 2-fluoro-5-nitroaniline with mercuric acetate and further with tellurium(IV) tetrabromide. Reaction of (4-amino-5-fluoro-2-nitrophenyl)tellurium(IV) tribromide with 4-hydroxyphenyl mercury(II) chloride gives asymmetrical diaryltellurium(IV) dibromide, whereas reaction of (4-amino-5-fluoro-2-nitrophenyl)mercury(II) chloride with phenol and 4-hydroxy benzaldehyde produces a new aryl mercury(II) chloride that contains the azomethine and azo groups. Reaction of aryl mercury(II) chloride with tellurium(IV) tetrabromide results in aryaltellurium(IV) tribromide furnished by the azomethine and azo groups. Reduction of unsymmetrical diaryltellurium(IV) dibromide and aryltellurium(IV) tribromide by hydrazine hydrate leads to the corresponding asymmetrical diaryltelluride and diarylditelluride. Structures of the new synthesized compounds are supported by FT-IR and 1H NMR spectra. Anti-bacterial activity of the new products has been tested against Klebsiella pneumonia Proteus, Escherichia coli, Pseudomonas spp., and Staphylococcus aureus. The compounds are characterized as highly active. The molecular structure level and energies of compounds have been computed through the Density Functional Theory (DFT).

Synthesis of Newer Mercury(II) Complexes of Meso-Tetraaryl-21,23-Dithiaporphyrins

Due to the larger size of hetero atom and poor binding with metals, N2X2 type of core modified porphyrins show lesser tendency to form metal complexes. Mercury(II) complexes of symmetrical and unsymmetrical meso-tetraaryl-21,23-dithiaporphyrins are synthesized and characterized by the reaction of corresponding meso-tetraaryl-21,23-dithiaporphyrins with mercuric acetate in chloroform/methanol. These mercury complexes are well characterized by their UV-Visible spectra, fluorescence spectra, 1H NMR, 13C NMR and elemental analysis. Soret bands of mercury complex of unsymmetrical 5,20-bis-(4′-methoxyphenyl)-10,15-bisphenyl-21,23-dithiaporphyrin appeared at 442 nm and 462 nm whereas Q band appeared at 516 nm, 560 nm, 620 nm and 714 nm. Appearance of four Q bands is characteristic for this mercury complex of N2X2 type of core modified porphyrins. Mercury complex of unsymmetrical 5,20-bis-(4′-methoxyphenyl)-10,15-bisphenyl-21,23dithiaporphyrin is an excellent fluorescent molecule and showed fluorescence spectrum at 722 nm. These core modified porphyrin complexes provides a good coordination examples of mercury complexes of 21,23-dithiaporphyrins that can be used in sensing applications.

Synthesis and characterization of new mixed ligand complexes of Zn (II) and Hg (II) with dithiocarbamate and phosphines

Complexes of the type [M (Et2DTC)2]2 [M= Zn(1) or Hg(2)] were prepared from the reaction of mercury acetate or zinc acetate with sodium diethyldithiocarbamate trihydrate (NaEt2DTC.3H2O) in (1:2) molar ratio (metal: ligand) in mixture of MeOH and H2O as a solvent. Treatment equal molar of (1) or (2) with diphosphine ligands {where diphos: bis (diphenylphosphino) methane (dppm), 1,2-bis (diphenylphosphino) ethane (dppe) and 1,3-Bis (diphenylphosphino) propane (dppp)} afforded complexes of the type [Zn(Et2DTC)2(dppeO)] (3); [Zn(Et2DTC)2(dpppS)] (4a); [Zn(Et2DTC)2(dppp)] (4b); [Hg(Et2DTC)2(dppm)] (6a); [Hg(Et2DTC)2(µ-dppm)]2(6b); [Hg(Et2DTC)2(dppe)](7) and [Hg(Et2DTC)2(dppp)](8), or with two moles of triphenylphosphine (PPh3) afforded a complexes of the type [M(κ1-Et2DTC)2(PPh3)2] (5a, 9a) and [M(κ2-Et2DTC)2(PPh3)2] (5b, 9b) {M= Zn, Hg}. The prepared complexes were fully characterized by different technics such as IR, NMR (1H and 31P) spectroscopy, elemental analysis, and molar conductivity. Characterization data showed that the (Et2DTC) ligand in all of the prepared complexes was coordinated with metal through the sulfur atoms of CSS- group. The geometry of the complexes (1-9) were tetrahedral around the Zn(II) and Hg(II) ions, except isomers 5b and 9b are octahedral geometry. .

Physiological and SCoT molecular analyses of Tomato (Solanum lycopersicum M.) plants in response to hazardous irrigation: wastewater, copper acetate and mercuric acetate

Physiological and SCoT molecular analyses of Tomato (Solanum lycopersicum M.) plants in response to hazardous irrigation: wastewater, copper acetate and mercuric acetate

Practical method for air sampling and analysis of some natural gas odorant

In this study, a method was presented for sampling and analysis of co-exposure to gas odorants such as methyl ethyl sulphide (MES), dimethyl sulphide (DMS) and tert-butyl mercaptane (TBM). An impregnated fibre glass with mercuric acetate was used for air sampling of odorants. In this study, odorant assessment was optimised with respect to the mercuric acetate, type of solution for odorant releasing and type of solvent for liquid-liquid extraction. Air sampling simulation was provided by standard preparation in tedlar bag. Odorants were analysed by gas chromatography equipped with mass spectrometry. Odorants released from 7% impregnated filters by 20% hydrochloric acid. MES, DMS and TBM were extracted by dichloroethane. Inter-day and intra-day coefficients variation was found to be lower than 11 by the recovery higher than 94%. According to the results of the recent study, a practical and reliable method was presented for air sampling and analysis of DMS, MES and TBM. [Received: October 8, 2019; Accepted: April 23, 2020]

The use of probiotic Lactobacillus plantarum and Lactobacillus bifermentans as antidote of mercury metal (Hg) to the mice Rattus norvegicus

Methyl mercury is a sort of most toxic mercury which was long since used by society in various fields. Methyl mercury is produced by a methilation process of anorganic mercury compound by metanogenic bacteria in aquatic sediment. The existence of excessive methyl mercury in the environment will be dangerous if entering the body of living beings. The aim of this research was to know the potential of probiotic bacteria spesies Lactobacillus plantarum and Lactobacillus bifermentans (in vivo) as antidote of mercury (Hg) poisoning to the experimental mice (Rattus norvegicus L.) after contacting methyl mercury acetate. This research used 5 various treatments where each of them conducted in 3 times repetition. The treatment which was used as follows; aquadest (positive control), mercury acetate 2 ppm (negative control), and probiotic bacteria Lactobacillus bifermentans; Lactobacillus plantarum; and also mixture culture of them. The observed parameter is the concentration of methyl mercury in blood and also through morphology observation qualitatively. The result of research shows that the giving of probiotic bacteria gives the real effect in decreasing the concentration of methyl mercury in blood. The best potential of probiotic bacteria as an antidote is Lactobacillus bifermentans because it can reduce the concentration of giving methyl mercury around 90,7 %.

New Salicylanilide-Hg(II) complexes with phosphine ligands, Synthesis and spectroscopic investigation

A new complex of the type [Hg(k2-Saln)2] (1) was prepared from the reaction of mercury acetate and salicylanilide (HSaln) in (1:2) molar ratio EtOH as a solvent with presence an Et3N as a base. Treatment of complex (1) with diphosphine {where diphos: dppe, dppp, dppb dppf and dppmS2} in 1:1) (complex: diphos) molar ratio afforded a complexes of the types [Hg(k1-Saln)2(diphos)] (2-6),where as a complexes of the types [Hg(k1-Saln)2(phos)2] (7,8) when treatment of complex(1) with two moles of monophosphine (PPh3 or SPPh3). The prepared complexes were fully characterization by many technical such as elemental analysis, molar conductivity, infrared spectroscopy, and nuclear magnetic resonance (1H and 31P). In complex (1) the (Saln-) was bonded as bidentate chelating ligand through the oxygen atoms of the carbonyl and deprotonated hydroxyl group, whereas bonded as monodentate ligand through the oxygen atom of deprotonated hydroxyl group in all other complexes (2-8). The geometry of the complexes (1-8) is a tetrahedral around the mercury (II) ion.
 
 http://dx.doi.org/10.25130/tjps.24.2019.086

New Salicylanilide-Hg(II) complexes with phosphine ligands, Synthesis and spectroscopic investigation

A new complex of the type [Hg(k2-Saln)2] (1) was prepared from the reaction of mercury acetate and salicylanilide (HSaln) in (1:2) molar ratio EtOH as a solvent with presence an Et3N as a base. Treatment of complex (1) with diphosphine {where diphos: dppe, dppp, dppb dppf and dppmS2} in 1:1) (complex: diphos) molar ratio afforded a complexes of the types [Hg(k1-Saln)2(diphos)] (2-6),where as a complexes of the types [Hg(k1-Saln)2(phos)2] (7,8) when treatment of complex(1) with two moles of monophosphine (PPh3 or SPPh3). The prepared complexes were fully characterization by many technical such as elemental analysis, molar conductivity, infrared spectroscopy, and nuclear magnetic resonance (1H and 31P). In complex (1) the (Saln-) was bonded as bidentate chelating ligand through the oxygen atoms of the carbonyl and deprotonated hydroxyl group, whereas bonded as monodentate ligand through the oxygen atom of deprotonated hydroxyl group in all other complexes (2-8). The geometry of the complexes (1-8) is a tetrahedral around the mercury (II) ion.