Sulfur fixation on bagasse activated carbon by chemical treatment and its effect on acid dye adsorption

Heteroatoms are known to introduce specific surface functionalities that can enhance the adsorption properties of carbons. Sulfur fixation on bagasse-activated carbon was conducted by a low temperature chemical treatment with sulfuric acid followed by physical activation with CO₂ at 900?°C. The effect of sulfur fixation on the surface chemical properties of bagasse-activated carbons were investigated and on their subsequent acid dye removal (CIBA AB80) behavior. Surface chemical development were examined and followed using Fourier transform infrared spectroscopy (FTIR), heteroatom analysis and carbon surface acidity. Functional group stability with thermal treatment was also investigated. The textural properties of the activated carbons were characterized by nitrogen adsorption. Chemical pre-treatment and gasification was able to fix up to 0.2 wt% of sulfur on the activated carbon. Although the sulfur fixed by chemical treatment is low, this method introduced several advantages in comparison to fixation by thermal methods. The chemical method did not interfere with the textural development of the carbon, as found in thermal methods. In addition, the surface chemistry generated by these levels of sulfur groups was sufficient to increase the uptake of acid blue dyes by more than 700% based on adsorption capacities normalized by the surface area of the carbon.     

Quantitative determination of acetylsalicylic acid and acetaminophen in tablets by FT-Raman spectroscopy

A procedure for quantitative determination of acetylsalicylic acid and acetaminophen in pharmaceuticals by PLS (partial least squares) and PCR (principal component regression) treatment of FT (Fourier transform)-Raman spectroscopic data is proposed. The proposed method was tested on powdered samples. Three chemometric models were built: the first, for samples consisting of an active substance diluted by lactose, starch and talc; the second, in which a simple inorganic salt was applied as an internal standard and additions were not taken into account; and the third, in which a model was constructed for a commercial pharmaceutical, where all constituents of the tablet were known. By utilising selected spectral ranges and by changing the chemometric conditions it is possible to carry out fast and precise analysis of the active component content in medicines on the basis of the simplified chemometric models. The proposed method was tested on five commercial tablets. The results were compared with data obtained by intensity ratio and pharmacopoeial methods. To appraise the quality of the models, the relative standard error of predictions (RSEPs) were calculated for calibration and prediction data sets. These were 0.7-2.0% and 0.8-2.3%, respectively, for the different PLS models. Application of these models to the Raman spectra of commercial tablets containing acetylsalicylic acid gave RSEP values of 1.3-2.0% and a mean accuracy of 1.2-1.7% with a standard deviation of 0.6-1.2%.     

Humic acid adsorption on fly ash and its derived unburned carbon

Fly ash is solid waste from combustion process, containing oxide minerals and unburned carbon. In this investigation, fly ash has been separated into metal oxide mineral section and unburned carbon. The fly ash with different contents of unburned carbon was employed for humic acid adsorption to investigate the influence of unburned carbon on adsorption. It is found that metal oxides and unburned carbon in fly ash exhibit significant difference in humic acid adsorption. The unburned carbon plays the major role in adsorption. Higher content of unburned carbon in fly ash results in higher surface area and thus higher humic acid adsorption. Fly ash and unburned carbon exhibit adsorption capacity of humic acid of 11 and 72 mg/g, respectively, at 30 degrees C, pH 7. Humic acid adsorption is also affected by ion strength, pH, and temperature. The thermodynamic calculations indicate that the adsorption is endothermic nature with DeltaH(0) and DeltaS(0) as 5.79 kJ/mol and 16.0 J/K mol, respectively.     

Characterization and sensing properties of a carbon nanotube paste electrode for acetaminophen

New separation and preconcentration procedures based on the coprecipitation of Fe(III) and Pb(II) ions with Cu(II) salicylaldoxime coprecipitant and of Cu(II) with Ni(II) salicylaldoxime coprecipitant were studied comparatively. The coprecipitation conditions for each method, such as the effect of the pH, the amounts of carrier elements and reagent, sample volume and matrix effects were examined in detail. The determinations of analyte ions were performed by flame AAS. Under optimised conditions the detection limits of the methods (3s/b) were 1.58, 3.56 and 1.32 μg L^?1 for iron(III), lead(II) an copper(II), respectively. The precision (as RSD %) of the methods was ≤3.2%. Each method was validated by both spiked tap water, dam water samples and by the analysis of certified reference material (TMDA-54.4 fortified lake water). It was found that the recovery of Fe(III), Pb(II) and Cu(II) from the water samples was ≥90%.     

Anodic oxidation of hydrazine at carbon nanotube powder microelectrode and its detection

Carbon nanotube powder microelectrodes (CNTPMEs) were used to study the anodic oxidation of hydrazine at Carbon nanotube (CNT)-the novel carbon material. It was found that the electrochemical behaviours were greatly improved at CNTs, indicating that the anodic oxidation could be catalyzed at CNTs. The kinetics parameters of this process were calculated, the heterogeneous electron transfer rate constant k was 0.0019 cm s(-1), (1-alpha)n(alpha) was 0.22. The CNTPMEs were also found with high sensitivity for hydrazine detection, could be used as hydrazine sensors.     

Wax-impregnated carbon paste electrode modified with mercuric oxalate for the simultaneous determination of heavy metal ions in medicinal plants and Ayurvedic tablets.

A wax-impregnated carbon paste electrode with mercury oxalate as the bulk modifier is found to be suitable for the determination of heavy metal ions by differential pulse anodic stripping voltammetry. The contents of binder and modifier have been optimized, until they showed low background current and easy renewability. The bulk-modified electrode is applied for the simultaneous determination of Zn, Cd, Pb and Cu in medicinal plants and Ayurvedic tablets (Liv 52). The results obtained have been validated with HMDE and AAS and are found to be comparable.     

The determination of acetaminophen using a carbon nanotube:graphite-based electrode

The oxidation of acetaminophen was studied at a glassy carbon electrode modified with multi-walled carbon nanotubes and a graphite paste. Cyclic voltammety, differential pulse voltammetry and square wave voltammetry at various pH values, scan rates, and the effect of the ratio of nanotubes to graphite were investigated in order to optimize the parameters for the determination of acetaminophen. Square wave voltammetry is the most appropriate technique in giving a characteristic peak at 0.52 V at pH 5. The porous nanostructure of the electrode improves the surface area which results in an increase in the peak current. The voltammetric response is linear in the range between 75 and 2000 ng.mL^?1, with standard deviations between 0.25 and 7.8%, and a limit of detection of 25 ng.mL^?1. The method has been successfully applied to the analysis of acetaminophen in tablets and biological fluids.     

Possibilities of powder X-ray diffraction methods in determining structural characteristics of carbon materials

The possibilities of using powder X-ray diffraction methods in the study of carbon materials are discussed. To determine the phase composition of the crystalline materials the X-ray phase analysis is employed; the real structure is established by the harmonic analysis of diffraction profiles; the structural features and phase composition of the nanomaterials are found by the radial electron density distribution function.     

新铜试剂分光光度法测定片剂中的对乙酰氨基酚含量及其反应机理的研究

使用分光光度法测定扑热息痛中主要化学成分对乙酰氨基酚的含量。结果表明:在0.04~8.00 mg·L-1范围内对乙酰氨基酚含量与吸光度(A)呈良好的线性关系,其线性方程:A=0.1210c+0.0261,相关系数r=0.9968。表观摩尔吸光系数为1.8×104 L·mol-1·cm-1,平均回收率为100.2%,相对标准偏差RSD为1.51%。该实验所用仪器简单,且操作方便、快速。用该方法测定扑热息痛片剂对乙酰氨基酚的含量,取得了较好的效果。     

Thermodynamic parameters of adsorption of adamantane and its derivatives on graphitized thermal carbon black

The adsorption equilibrium constants for adamantane, 1-fluoro-, 1-chloro-, 1,3-difluoro-, 1,3-dichloro-, 1,3-dibromo-, and 1-hydroxyadamantane, and methyl 1-adamantyl ketone were determined by gas chromatography. The results were compared with molecular statistical calculations based on the known atomic-atomic potentials of the interaction of atoms of the sorbate molecule with the C atom of graphitized thermal carbon black (GTCB). The experimental adsorption heats exceed the calculated values by 3-10 kJ mol^-1. The reasons for this divergence are discussed. The changes in the adsorption entropy show that the molecules of the studied compounds form a layer of the ideal dimeric gas on the GTCB surface upon adsorption.     

Nitrogen-doped carbon nanotubes modified with gold nanoparticles for simultaneous analysis of N-acetylcysteine and acetaminophen

A novel film consisting of nitrogen-doped multi-walled carbon nanotubes modified with gold nanoparticles (further denoted as N-MWCNTs/AuNPs) was fabricated and applied for the simultaneous electrochemical analysis of N-acetylcysteine (NAC) and acetaminophen (AC) in phosphate buffer solution (PBS, pH 7.0). The fabricated film exhibits powerful response towards simultaneous analysis of NAC and AC followed by well-separated cyclic voltammetric waves (～440 mV). The oxidation peak currents of NAC and AC increase linearly with their concentrations in the ranges of 0.100–1.510 mM and 0.063–0.190 mM, respectively. The detection limits of N-MWCNTs/AuNPs towards NAC and AC were estimated to be 3.0 and 0.35 μM, respectively. The good catalytic activity, the high detection ability, and the great stability of N-MWCNTs/AuNPs verify that such composite materials are extremely promising for the construction of biosensors.     

Simultaneous high-performance liquid chromatographic stability-indicating analysis of acetaminophen and codeine phosphate in tablets and capsules

A high-performance liquid chromatographic method has been developed for the simultaneous determination of acetaminophen and codeine phosphate for product stability studies, and release and dissolution testing of tablets and capsules. The reversed-phase method utilizes UV detection at 214 nm, a C18 column and requires a maximum of 10 min per analysis. The method has been validated for use with products containing as much as 500 mg of acetaminophen and as little as 7.5 mg of codeine phosphate. The known potential degradation products, p-aminophenol, codeine N-oxide, and codeinone are separated for quantitation simultaneous with the parent compounds. The method has been shown to be linear, reproducible, specific, sensitive and rugged.     

活性炭吸附CO2与其微孔体积的关系

对五种活性炭样品进行液氮温度下的N2吸附、碘吸附测定和冰点下的CO2吸附表征。结果表明,碘吸附值测定法和基于N2吸附等温线的BET方程、D-R方程,孔结构参数都不能正确反映活性炭对CO2的吸附特性;由CO2吸附等温线得到的D A模型参数也不适合分析活性炭吸附CO2特性;CO2吸附等温线的密度泛函理论（DFT）分析结果表明,CO2在活性炭上的吸附发生在极微孔内,DFT分析的微孔孔容与吸附等温线反映的吸附性能完全一致。因此,根据CO2吸附等温线的DFT模型是准确反映活性炭吸附CO2特性的表征分析方法。     

Potassium bromate modification of the granular activated carbon and its effect on nickel adsorption

Granular Activated Carbon (GAC), a commercial adsorbent for the removal of heavy metals was treated chemically with potassium bromate for it’s surface modification and it’s adsorption capacity was investigated with nickel ions. There was an increase in the adsorption capacity of the modified carbon by 90–95% in comparison to the raw granular activated carbon towards nickel ion adsorption. Potassium Bromate oxidation treatment was employed for a period of about 30 mins initially followed by 60 mins and the oxidized carbons were adsorbed with nickel ions. Metal sorption characteristics of as received and modified activated carbons were measured in batch experiments. Batch adsorption was successfully modeled by Langmuir Isotherm Model which indicates monolayer adsorption. The adsorption isotherms also fit well to the Freundlich Model. Effects of pH of initial solution, time of oxidation and mode of treatment on the adsorption process were studied. Experimental results showed that metal uptake increased with an increase in pH and oxidation time. The samples were characterized by Scanning Electron Microscope (SEM) studies and surface area analyzer.     

Heats of adsorption and adsorption heterogeneity for methane, ethane, and carbon dioxide in MCM-41

We report the adsorption isotherms and the isosteric heats of adsorption of pure methane, ethane, and CO2 and a mixture of methane and CO2 in the periodic mesoporous silica MCM-41 using a multicomponent adsorption calorimeter of the Tian-Calvet type, looking in particular at the degree of heterogeneity in the adsorption of these species. The adsorption of methane and ethane in MCM-41 was found to be essentially homogeneous, while the adsorption of pure CO2 and of CO2 from a CO2/methane mixture was found to be significantly heterogeneous, reflecting the electrostatic interactions between CO2 and the adsorbent.     

Synthesis and characterization of ordered mesoporous carbon as electrocatalyst for simultaneous determination of epinephrine and acetaminophen

In this research, we report an easy method for synthesis of ordered mesoporous carbon (OMC) with hexagonal arrays of tubes (CMK-5). The synthesized OMC was characterized using X-ray diffraction (XRD), scanning electronic microscopy (SEM) and nitrogen sorption isotherms techniques. Due to the large surface area and high conductivity of OMC, OMC-modified glassy carbon (OMCs/GC) electrode was prepared. The unique electrochemical activity of OMCs/GC electrode was illustrated using cyclic voltammetry (CV) and electron impedance spectroscopy (EIS) in which OMC showed a faster electron transfer rate, as compared with glassy carbon electrode. The electrochemical behavior of epinephrine (EN) and acetaminophen (AP) at OMC/GC electrode was also investigated using cyclic voltammetry. The OMC/GC electrode exhibited high electrocatalytic activities toward oxidation of EN and AP and displayed good voltammetric peak separation between them. In differential pulse voltammetry technique, both EN and AP give sensitive oxidation peaks at 120?mV and 320?mV, respectively. Therefore, investigated method was applied for simultaneous determination of EN and AP. AP and EN give linear response over the range of 0.2–15?μM and 4–100?μM, respectively. The lower detection limits were found to be 0.07?μM for AP and 0.94?μM for EN.     

Correlation of fractal pore-size distribution of activated carbon fiber with its adsorption for low concentration benzene vapor

Fractal pore-size distribution K(x) is given based on J(x) function proposed by Jaronic. Activated carbon fibers (ACF) with different surface areas are characterized by using two functions mentioned above. The present work studies the fractal pore-size distribution of ACF and adsorption isotherms of nonpolar benzene vapor on ACF, and thereby reveals the correlation between them.