Biomethane Production in an AnSBBR Treating Wastewater from Biohydrogen Process

An anaerobic sequencing batch reactor containing immobilized biomass (AnSBBR) was used to produce biomethane by treating the effluent from another AnSBBR used to produce biohydrogen from glucose- (AR-EPHG) and sucrose-based (AR-EPHS) wastewater. In addition, biomethane was also produced from sucrose-based synthetic wastewater (AR-S) in a single AnSBBR to compare the performance of biomethane production in two steps (acidogenic and methanogenic) in relation to a one-step operation. The system was operated at 30 °C and at a fixed stirring rate of 300 rpm. For AR-EPHS treatment, concentrations were 1,000, 2,000, 3,000, and 4,000 mg chemical oxygen demand?(COD)?L^?1 and cycle lengths were 6 and 8 h. The applied volumetric organic loads were 2.15, 4.74, 5.44, and 8.22 g COD L^?1 day^?1. For AR-EPHG treatment, concentration of 4,000 mg COD L^?1 and 4-h cycle length (7.21 g COD L^?1 day^?1) were used. For AR-S treatment, concentration was 4,000 mg COD L^?1 day^?1 and cycle lengths were 8 (7.04 g COD L^?1 day^?1) and 12 h (4.76 g COD L^?1 day^?1). The condition of 8.22 g COD L^?1 day^?1 (AR-EPHS) showed the best performance with respect to the following parameters: applied volumetric organic load of 7.56 g COD L^?1 day^?1, yield between produced methane and removed organic material of 0.016 mol CH₄?g COD^?1, CH₄ content in the produced biogas of 85 %, and molar methane productivity of 127.9 mol CH₄?m^?3 day^?1. In addition, a kinetic study of the process confirmed the trend that, depending on the biodegradability characteristics of the wastewaters used, the two-step treatment (acidogenic for biohydrogen production and methanogenic for biomethane production) has potential advantages over the single-step process.     

Anaerobic Digestion of Sugarcane Vinasse Through a Methanogenic UASB Reactor Followed by a Packed Bed Reactor

The anaerobic treatment of raw vinasse in a combined system consisting in two methanogenic reactors, up-flow anaerobic sludge blanket (UASB) + anaerobic packed bed reactors (APBR), was evaluated. The organic loading rate (OLR) was varied, and the best condition for the combined system was 12.5 kg COD m^?3day^?1 with averages of 0.289 m³ CH₄ kg COD r^?1for the UASB reactor and 4.4 kg COD m^?3day^?1 with 0.207 m³ CH₄ kg COD r^?1 for APBR. The OLR played a major role in the emission of H₂S conducting to relatively stable quality of biogas emitted from the APBR, with H₂S concentrations <10 mg L^?1. The importance of the sulphate to COD ratio was demonstrated as a result of the low biogas quality recorded at the lowest ratio. It was possible to develop a proper anaerobic digestion of raw vinasse through the combined system with COD removal efficiency of 86.7% and higher CH₄ and a lower H₂S content in biogas.     

Effects of Organic Loading, Influent Concentration, and Feed Time on Biohydrogen Production in a Mechanically Stirred AnSBBR Treating Sucrose-Based Wastewater

An anaerobic sequencing batch biofilm reactor (AnSBBR—total volume 7.5 L; liquid volume 3.6 L; treated volume per cycle 1.5 L) treated sucrose-based wastewater to produce biohydrogen (at 30 °C). Different applied volumetric organic loads (AVOL of 9.0, 12.0, 13.5, 18.0, and 27.0 kg COD m^?3 day^?1), which were varied according to the influent concentration (3,600 and 5,400 mg COD L^?1) and cycle length (4, 3, and 2 h), have been used to assess the following parameters: productivity and yield of biohydrogen per applied and removed load, reactor stability, and efficiency. The removed organic matter (COD) remained stable and close to 18 % and carbohydrates (sucrose) uptake rate remained between 83 and 97 % during operation. The decrease in removal performance of the reactor with increasing AVOL, by increasing the influent concentration (at constant cycle length) and decreasing the cycle lengths (at constant influent concentrations), resulted in lower conversion efficiencies. Under all conditions, when organic load increased there was a predominance of acetic, propionic, and butyric acid as well as ethanol. The highest concentration of biohydrogen in the biogas (24–25 %) was achieved at conditions with AVOL of 12.0 and 13.5 kg COD m^?3 day^?1, the highest daily production rate (0.139 mol H₂?day^?1) was achieved at AVOL of 18.0 kg COD m^?3 day^?1, and the highest production yields per removed and applied load were 2.83 and 3.04 mol H₂?kg SUC^?1, respectively, at AVOL of 13.5 kg COD m^?3 day^?1. The results indicated that the best productivity tends to occur at higher organic loads, as this parameter involves the “biochemical generation” of biogas, and the best yield tends to occur at lower and/or intermediate organic loads, as this parameter involves “biochemical consumption” of the substrate.     

Simultaneous Analysis of Sugars and Polyphenols in Tobacco by CZE with Amperometric Detection Based on a Cu2O/MWCNT-COOH Composite Electrode

A composite electrode was fabricated from Cu₂O powder, carboxyl-functionalized multi-wall carbon nanotubes (MWCNT-COOH), and paraffin oil in the proportions 51:17:32 (w/w). This composite electrode was used for amperometric detection (CZE–AD) in simultaneous capillary zone electrophoretic analysis of chlorogenic acid, rutin, sucrose, glucose, mannose, and fructose in tobacco samples. Under the optimum conditions, the six analytes could be separated in 100 mmol L^?1 NaOH buffer within 30 min. Good linearity was achieved in the range 1 × 10^?7–1 × 10^?4 mol L^?1 for the two polyphenols and 5 × 10^?6–1 × 10^?3 mol L^?1 for the four sugars. The detection limits (S/N = 3) for the polyphenols and sugars were as low as 10^?8 mol L^?1 and 10^?6 mol L^?1, respectively.     

Simultaneous Determination of Acetaminophen, Caffeine, and Chlorphenamine Maleate in Paracetamol and Chlorphenamine Maleate Granules

A simple and rapid HPLC method using phenacetin (PHN) as internal standard has been developed for simultaneous determination of acetaminophen, caffeine, and chlorphenamine maleate in the product compound paracetamol and chlorphenamine maleate granules. Separation and quantitation were achieved on a 250 mm × 4.6 mm, 5 μm particle, C₁₈ column. The mobile phase was methanol 0.05 mol L^?1 aqueous KH₂PO₄ solution, 45:55 (v/v), containing 0.1% triethylamine and adjusted to pH 3.6 by addition of phosphoric acid; the flow rate was 1.0 mL min^?1. Detection of all compounds was by UV absorbance at 260 nm and elution of the analytes was achieved in less than 12 min. The linearity, accuracy, and precision of the method were acceptable to good over the concentration ranges 6.4–153.6 μg mL^?1 for acetaminophen, 5.0–120.0 μg mL^?1 for caffeine, and 9.6–230.4 μg mL^?1 for chlorphenamine maleate.     

Determination of Veterinary Pharmaceuticals in Production Wastewater by HPTLC-Videodensitometry

An SPE-HPTLC method for simultaneous identification and quantification of seven pharmaceuticals in production wastewater was optimized and validated. The studied compounds were enrofloxacine, oxytetracycline, trimethoprim, sulfamethazine, sulfadiazine, sulfaguanidine and penicillin G/procaine. The method involves solid-phase extraction on hydrophilic-lipophilic balance cartridges with methanol and HPTLC analysis of extracts on CN modified chromatographic plates followed by videodensitometry at 254 and 366 nm. Optimization of chromatographic separation was performed by systematic variation of the mobile phase composition using genetic algorithm approach and the optimum mobile phase composition for TLC separation was 0.05 M H₂C₂O₄:methanol = 0.81:0.19 (v/v). Linearity of the method was demonstrated in the ranges from 1.5 to 15.0 μg L⁻¹ for enrofloxacine, 100–500 μg L⁻¹ for oxytetracycline, 150–600 μg L⁻¹ for trimethoprim, 300–1100 μg L⁻¹ for sulfaguanidine and 100–400 μg L⁻¹ for sulfamethazine, sulfadiazine and penicillin G/procaine with coefficients of determination higher than 0.991. Mean recoveries ranged from 74.6 to 117.1% and 55.1 to 108.0% for wellspring water and production wastewater, respectively. Only sulfaguanidine showed lower results. The described method has been applied to the determination of pharmaceuticals in wastewater samples from pharmaceutical industry.     

Sensitive detection of sulfanilamide by redox process electroanalysis of oxidation products formed in situ on glassy carbon electrode

This paper reported a simple method for sulfanilamide determination by redox process electroanalysis of oxidation products (SFDox) formed in situ on glassy carbon electrode. The CV experiments showed a reversible process after applied E _acc = + 1.06 V and t _acc = 1 s, in 0.1 mol L^?1 BRBS (pH = 2.0) at 50 mV s^?1. Different voltammetric scan rates (from 10 to 450 mV s^?1) suggested that the redox peaks of SFDox on the glassy carbon electrode (GCE) is an adsorption-controlled process. Square-wave voltammetry (SWV) method optimized conditions showed a linear response to SFD from 3.00 to 250.0 μmol L^?1 (R = 0.998) with a limit of detection of 0.638 μmol L^?1 and limit of quantification of 2.0 μmol L^?1. The developed the SWV method was successfully used in the determination of SFD pharmaceutical formulation and human serum. The SFD quantification results in pharmaceutical obtained by SWV-GCE were comparable to those found by official analytical protocols.     

Chemiluminescent Determination of Vitamin B12 Using Charge Coupled Device (CCD)

A method was developed for the determination of vitamin B₁₂ based on the enhancement of cobalt (II) on the chemiluminescence (CL) reaction between luminol and percarbonate (powerful source of hydrogen peroxide). The release of cobalt (II) from the vitamin B₁₂ was reached by a simple and fast microwave digestion (20 s microwave digestion time and a mix of nitric acid and hydrogen peroxide). A charge coupled device (CCD) photodetector, directly connected to the cell, coupled with a simple continuous flow system was used to obtain the full spectral characteristics of cobalt (II) catalyzed luminol-percarbonate reaction.

The optima experimental conditions were established: 8.0 m mol L^?1 luminol in a 0.075 mol L^?1 carbonate buffer (pH 10.0) and 0.15 mol L^?1 sodium percarbonate, in addition to others experimental parameters as 0.33 mL s^?1 flow rate and 2 s integration time, were the experimental conditions which proportionate the optimum CL emission intensity. The emission data were best fitted with a second-order calibration graph over the cobalt (II) concentration range from 4.00 to 300 µ g L^?1 (r² = 0.9990), with a detection limit of 0.42 µ g L^?1. The proposed method was successfully applied to the determination of vitamin B₁₂ in pharmaceuticals.     

Optimized solid phase extraction based on diethyldithiocarbamate-coated Fe3O4 magnetic nanoparticles followed by ICP-OES for determination of Cd(II) and Ni(II) in rice and water samples

In the present study, application of Fe₃O₄ magnetic nanoparticles (MNPs) coated with diethyldithiocarbamate as a solid-phase sorbent for extraction of trace amounts of cadmium (Cd²⁺) and nickel (Ni²⁺) ions by the aid of ultrasound was investigated. The analytes were determined by inductively coupled plasma-optical emission spectroscopy. Fe₃O₄ MNPs were prepared by solvothermal method and characterized with dynamic light scattering, scanning electron microscope and X-ray diffraction. Response surface methodology was used for optimization of the extraction process and modeling the data. The optimal conditions obtained were as follows: chelating agent, 1.2 g L^?1; pH, 6.13; sonication time, 13 min and Fe₃O₄ MNPs, 10.3 mg. The calibration curves were linear over the concentration range of 1–1,000 μg L^?1 for Cd²⁺ and 2.5–1,000 for Ni²⁺ with the determination coefficients (R ²) of 0.9997 and 0.9995, respectively. The limits of detection were 0.27 μg L^?1 for Cd²⁺ and 0.76 μg L^?1 for Ni²⁺. The relative standard deviations (n = 7, C = 200 μg L^?1) for determination of Cd²⁺ and Ni²⁺ were 2.0 and 2.7 %, respectively. The relative recoveries of the analytes from tap, river and lagoon waters and rice samples at the spiking level of 10 μg L^?1 were obtained in the range of 95–105 %.     

Determination of trace amounts of plutonium in low-active liquid wastes from spent nuclear-fuel reprocessing plants by flow injection-based solid-phase extraction/electrochemical detection system

A flow injection-based electrochemical detection system coupled to a solid-phase extraction column was developed for the determination of trace amounts of plutonium in low-active liquid wastes from spent nuclear-fuel reprocessing plants. The oxidation state of plutonium in a sample solution was adjusted to Pu(VI) by the addition of silver(II) oxide. A sample solution was made up in 3 mol L^?1 HNO₃ and loaded onto a column packed with UTEVA^® with 3 mol L^?1 HNO₃ as the carrier. Plutonium(VI) was adsorbed onto the resin, and interfering elements were removed by rinsing the column with 3 mol L^?1 HNO₃. Subsequently, the adsorbed Pu(VI) was eluted with 0.01 mol L^?1 HNO₃, and then introduced directly into the flow-through electrolysis cell with boron-doped diamond electrode. The eluted Pu(VI) was detected by an electrochemical amperometric method at a working potential of 0.1 V (vs. Ag/AgCl). The current produced on reduction of Pu(VI) was continuously monitored and recorded. The plutonium concentration was calculated from the relationship between the peak area and concentration of plutonium. The relative standard deviation of ten analyses was 1.1% for a plutonium solution of 25 μg L^?1 containing 50 ng of Pu. The detection limit calculated from three-times the standard deviation was 0.82 μg L^?1 (1.6 ng of Pu).     

Spectrophotometric Determination of Gold in Water and Ore with 2‐Carboxyl‐1‐Naphthalthiorhodanine

Abstract

This paper reports on the synthesis of a new chromogenic reagent, 2‐carboxyl‐1‐naphthalthiorhodanine (CNTR). A high sensitive, selective, and rapid method for the determination of gold based on the rapid reaction of gold with CNTR and the solid phase extraction of the colored chelate with a reversed phase polymer‐based C₁₈ cartridge was developed. In the presence of 0.05–0.5 mol L^?1 of phosphoric acid solution and emulsifier‐OP medium, CNTR reacts with gold to form a red chelate of a molar ratio 1∶3 (gold to CNTR). This chelate was enriched by the solid phase extraction with a polymer‐based C₁₈ cartridge and the retained chelate was eluted from the cartridge with dimethyl formamide (DMF). The enrichment factor of 100 was achieved. In the DMF medium, the molar absorptivity of the chelate is 1.35×10⁵ L · mol^?1 · cm^?1 at 540 nm. Beer's law is obeyed in the range of 0.01～2 µg mL^?1 in the measured solution. The relative standard deviation for 11 replicates sample of 0.5 µg L^?1 level is 2.05%. The detection limit, based on three times the standard deviation is 0.02 µg L^?1 in the original sample. This method was applied to the determination of gold in water and ore with good results.     

HPLC Analysis and Pharmacokinetic Study of Paeoniflorin after Intravenous Administration of a New Frozen Dry Powder Formulation in Rats

A simple and specific high performance liquid chromatographic (HPLC) method with UV detection using picroside II as the internal standard was developed and validated to determine the concentration of paeoniflorin in rat plasma and study its pharmacokinetics after an single intravenous administration of 40 mg kg^?1 paeoniflorin to Wistar rats. The analytes of interest were extracted from rat plasma samples by ethyl acetate after acidification with 0.05 mol L^?1 NaH₂PO₄ solution (pH 5.0). Chromatographic separation was achieved on an Agilent XDB C₁₈ column (250 × 4.6 mm I.D., 5 μm) with a Shim-pack GVP-ODS C₁₈ guard column (10 × 4.6 mm I.D., 5 μm) using a mobile phase consisting of acetonitrile–water–acetic acid (18:82:0.4, v/v/v) at a flow rate of 1.0 mL min^?1. The UV detection was performed at a wavelength of 230 nm. The linear calibration curves were obtained in the concentration range of 0.05–200.0 μg mL^?1 in rat plasma with the lower limit of quantification (LLOQ) of 0.05 μg mL^?1. The intra- and inter-day precisions in terms of % relative standard deviation (RSD) were lower than 5.7 and 8.2% in rat plasma, respectively. The accuracy in terms of % relative error (RE) ranged from ?1.9 to 2.6% in rat plasma. The extraction recoveries of paeoniflorin and picroside II were calculated to be 69.7 and 56.9%, respectively. This validated method was successfully applied to the pharmacokinetic study of a new paeoniflorin frozen dry power formulation. After single intravenous administration, the main pharmacokinetic parameters t _1/2, AUC_0-∞, CL_TOT, V _Z, MRT_0-∞ and V _ss were 0.739 ± 0.232 h, 43.75 ± 6.90 μg h mL^?1, 15.50 ± 2.46 L kg^?1 h^?1, 1.003 ± 0.401 L kg^?1, 0.480 ± 0.055 h and 0.444 ± 0.060 L kg^?1, respectively.     

Optimization of the Extraction Conditions and Simultaneous Quantification of Six Flavonoid Glycosides in Flos Chrysanthemi by RP-LC

A sensitive, accurate and reliable reversed-phase liquid chromatographic method coupled with DAD (278 nm) was established for simultaneous quantification of six compounds in 20 cultivars of Flos Chrysanthemi. The method was carried out by using a Kromasil 100-5 C₁₈ column with methanol–acetonitrile—1.414 × 10^?2 mol L^?1 aqueous phosphoric acid as a gradient mobile phase. The contents of the six flavonoid glycosides in Flos Chrysanthemi could be determined within 120 min. The linear calibration ranges for these were 0.42–126.00, 11.44–220.00, 0.53–530.00, 4.80–195.00, 11.00–220.00, and 0.12–200.00 μg mL^?1. Their recoveries were 95.33–105.33% with RSDs from 0.10 to 2.00%. Their lower limits of quantification were 0.420, 1.144, 0.250, 0.480, 0.242, and 0.120 μg mL^–1. The method can be used for analysis of the six flavonoid glycosides in Flos Chrysanthemi.     

Self-assembled sensor based on boron-doped diamond and its application in voltammetric analysis of picloram

A self-assembled sensor based on a boron-doped diamond was investigated as a sensitive tool for voltammetric analysis of a member of a pyridine herbicide family - picloram. A cyclic voltammetry and a differential pulse voltammetry were applied for investigation of the voltammetric behaviour and quantification of this herbicide. Picloram yielded one well-developed irreversible oxidation signal at a very positive potential about +1.5 V vs. Ag/AgCl/3 mol L^?1 KCl electrode in an acidic medium and 1 mol L^?1 H₂SO₄ was chosen as a suitable supporting electrolyte. Operating parameters of differential pulse voltammetry were optimized and the proposed voltammetric method provided a high repeatability (a relative standard deviation of 20 repeated measurements at a concentration level of picloram of 50 µmol L^?1 equaled to 2.58%), a linear concentration range from 2.5 to 90.9 µmol L^?1 and a low limit of detection (LD = 1.64 µmol L^?1). Practical usefulness of the ‘environmentally-green’ electrochemical sensor was verified by an analysis of spiked water samples with satisfactory recoveries.     

Molecularly imprinted stir bar sorptive extraction coupled with high-performance liquid chromatography for trace analysis of naphthalene sulfonates in seawater

In this paper, a novel molecularly imprinted polymer coated stir bar has been used to selectively extract naphthalene sulfonates (NS_s) directly from seawater sample. 1-Naphthalene sulfonic acid (1-NS) was used as template molecule. The effects of different parameters were optimized on the extraction efficiency and the optimum conditions were established as: the absorption and desorption times were fixed, respectively, at 10 and 15 min, stirring speed was 700 rpm, pH was adjusted to 4.1, amount of NaCl was 1 mol L^?1 and extraction process was performed at a temperature of 50 °C. The linear ranges were 2–250 µg L^?1 for 3,6-NDS-1-OH (1-naphthol-3,6-disulfonic acid), 4–250 µg L^?1 for 2-NS (2-naphthalene sulfonate) and 3–250 µg L^?1 for 1-NS. The detection limits were within the range of 0.32–0.95 µg L^?1. Under optimum conditions, the detection limits of the NSs were 0.84, 0.95 and 0.32 µg L^?1 with the enrichment factor of 117-, 41- and 77-fold for 2-NS, 1-NS, and 6-NDS-1-OH, respectively. The repeatability of the method was satisfactory (0.53 ≤ RSD ≤6.0 %, n = 10). The method has been successfully applied for the analysis of trace amounts of three naphthalene sulfonates in seawater of Chabahar Bay.     

Use of Surfactant as Mobile Phase Additive in LC for Simultaneous Determination of Metal-Pyrrolidine Dithiocarbamate Chelates

Reversed phase liquid chromatography using UV detection was developed for the simultaneous analysis of Hg(II), Pb(II), Cd(II), Ni(II), Fe(III) and V(V) ions after their complexation with pyrrolidine-dithiocarbamate (PDC). Optimum chromatographic conditions were a μ-Bondapak C₁₈ column and an isocratic mobile phase consisting of 40 mmol L^?1 SDS, 34 mmol L^?1 TBABr and 68% acetonitrile in 10 mmol L^?1 phosphate buffer pH 3.5. The separation of six PDC complexes was achieved within 8 min. Analytical performances and method validation were investigated. The detection limits ranged from 0.16 μg L^?1(Fe(III)) to 5.40 μg L^?1(Pb(II)). Recoveries obtained for all the studied samples including tap water, whole blood and vegetables were 72–98%. The results obtained from the proposed method were not significantly different compared to those obtained from atomic absorption spectrometry (P = 0.05).     

Preconcentration and spectrophotometric determination of trace amount of formaldehyde using hollow fiber liquid-phase microextraction based on derivatization by Hantzsch reaction

Formaldehyde is known as a highly toxic compound to humans and identified as a carcinogenic substance. In this study, Hantzsch reaction was utilized for the derivatization of trace amounts of formaldehyde in aqueous samples with acetylacetone in the presence of ammonia to form an extractable colored product named 3,5-diacetyl 1,4-dihydrolutidine (DDL) and its further extraction using two-phase hollow fiber liquid-phase microextraction. The main experimental variables affecting the extraction performance were investigated and optimized. Under the optimum conditions (sample volume 12 mL; reaction temperature 70 °C; ammonium acetate buffer solution 4 mL 0.1 mol L^?1; acetylacetone 5 mL 0.15 mol L^?1; solvent octanol, salt concentration 20% (w/v) NaCl; pH of donor phase 7.0; stirring speed 400 rpm and extraction time 30 min), the linear dynamic range, limit of detection (LOD as 3S _b/m) and relative standard deviation (RSD %) of the proposed method were obtained as 5–250 μg L^?1 (r ² = 0.9979), 3.6 μg L^?1 and 2.5%, respectively. Finally, the applicability of the proposed method was examined, and very good results were obtained. The results confirmed the applicability of the proposed method as a versatile, low-cost and sensitive preconcentration method for determination of low concentrations of formaldehyde in aqueous solutions.     

Thermochemical property of a microporous material for mixed metal borate of Li2Sr4B12O23

A pure mixed alkali–alkaline earth metal borate of Li₂Sr₄B₁₂O₂₃ with microporous structure has been synthesized by high-temperature solid state reaction, and characterized by XRD, FT-IR, TG techniques, and chemical analysis. The molar enthalpies of solution of Li₂Sr₄B₁₂O₂₃ in 1 mol L^?1 HCl(aq), and of SrCl₂·H₂O(s) in [1 mol L^?1 HCl + H₃BO₃ + LiCl·H₂O](aq) have been determined by microcalorimeter at 298.15 K, respectively. From these data and with the incorporation of the previously determined enthalpies of solution of H₃BO₃(s) in 1 mol L^?1 HCl(aq), and of LiCl·H₂O(s) in [1 mol L^?1HCl + H₃BO₃](aq), together with the use of the standard molar enthalpies of formation for SrCl₂·6H₂O(s), LiCl·H₂O(s), H₃BO₃(s), HCl(aq), and H₂O(l), the standard molar enthalpy of formation of ?(11,534.0 ± 10.0) kJ mol^?1 for Li₂Sr₄B₁₂O₂₃ was obtained on the basis of the appropriate thermochemical cycle.     

Flow‐Injection Spectrophotometric Determination of N‐acetylcysteine in Pharmaceutical Formulations with On‐Line Solid‐Phase Reactor Containing Zn(II) Phosphate Immobilized in a Polyester Resin

Abstract

A flow‐injection spectrophotometric procedure was developed for determining N‐acetylcysteine in pharmaceutical formulations. The sample was dissolved in deionized water and 400 µl of the solution was injected into a carrier stream of 1.0×10^?2 mol l^?1 sodium borate solution. The sample flowed through a column (70 mm length×2.0 mm i.d.) packed with Zn₃(PO₄)₂ immobilized in a polymeric matrix of polyester resin and Zn(II) ions were released from the solid‐phase reactor because of the formation of the Zn(II) (N‐acetylcysteine)₂ complex. The mixture merged with a stream of borate buffer solution (pH 9.0) containing 5.0×10^?4 mol l^?1 Alizarin red S and the Zn(II)Alizarin red complex formed was measured spectrophotometrically at 540 nm. The analytical curve was linear in the N‐acetylcysteine concentration range from 3.0×10^?5 to 1.5×10^?4 mol l^?1 (4.9 to 24.5 µg ml^?1) with a detections limit of 8.0×10^?6 mol l^?1 (1.3 µg ml^?1). The relative standard deviations (RSDs) were smaller than 0.5% (n=10) for solutions containing 5.0×10^?5 mol l^?1 (8.0 µg ml^?1) and 8.0×10^?5 mol l^?1 (13.0 µg ml^?1) of N‐acetylcysteine, and the analytical frequency was 60 determinations per hour. A paired t‐test showed that all results obtained for N‐acetylcysteine in commercial formulations using the proposed flow‐injection procedure and a comparative procedure agreed at the 95% confidence level.     

Determination of allura red using composites of water-dispersible reduced graphene oxide-loaded Au nanoparticles based on ionic liquid

A facile route for producing reduced graphene oxide (RGO)-loaded Au nanoparticles based on ionic liquids (IL) has been proposed, in which the as-prepared RGO can be dispersed stably in water. With the assistance of IL, Au nanoparticles were uniformly and densely absorbed on the surfaces of the IL functionalised reduced graphene oxide (IRGO), forming a new composite of IRGO/Au with high dispersibility. This IRGO/Au composite enhanced its electrochemical signal obviously in the measurement of allura red in foods and exhibited a wider linear response ranging from 0.297 (0.0006 μmol L^?1) to 99.3 μg L^?1 (0.2 μmol L^?1) with lower detection limit of 0.213 μg L^?1 (0.00043 μmol L^?1) at a signal-to-noise ratio of 3. To further study the practical applicability of the proposed sensor, the modified electrode was successfully applied to detect allura red in five kinds of common foods and the assay results were in a good agreement with the reference values detected by HPLC.