Supercapacitor performance of activated carbon derived from rotten carrot in aqueous,organic and ionic liquid based electrolytes

In this work, we report the synthesis of porous activated carbon (AC). AC was derived from rotten carrot, at different values of activating temperature under inert atmosphere, employing chemical activation method and ZnCl₂ as activation agent. On the basis of results observed by surface area and pore size analysis, effect of activation temperature on synthesized AC was determined. Other material properties such as morphology, thermal stability, vibrational response, and crystal structure of prepared AC were studied using standard techniques of material characterization. Further, the electrochemical performance of synthesized AC was studied as an electrode, in aqueous, organic and ionic liquid based electrolyte. It was found that the synthesized AC based electrode exhibits highest specific capacitance (135.5?F?g^?1 at 10?mHz) in aqueous electrolyte and highest specific energy (29.1?Wh?kg^?1 at 2.2?A?g^?1) and specific power (142.5?kW?kg^?1 at 2.2?A?g^?1) in ionic liquid based electrolyte. This shows the suitability of synthesized material for use in energy storage applications.     

Determination of concentrations of chromium and other elements in soil and plant samples from leather tanning area by Instrumental Neutron Activation Analysis

Chromium, one of the toxic elements, along with other elements has been determined in samples of soil and plant (leaves and seeds) from Jajmau Area, Kanpur district, India, which is irrigated with effluent waste water from leather tanning industries. Soil and plant samples were collected from these areas and analyzed by Instrumental Neutron Activation Analysis (INAA) using high flux reactor neutrons and high resolution gamma-ray spectrometry. Concentrations of fifteen elements in soil and five elements in plant samples were determined by relative method. Chromium concentrations were found to be in range of 45–3,900 mg kg^?1in soil samples and 14–83 mg kg^?1 in plant samples. This study showed that Cr is present in significant amounts, in the soil as well as in the plant samples, near to the leather tanning area. As a part of quality control work, IAEA reference material (RM) SL-3 and NIST standard reference material (SRM) 1645 were analyzed and the quality of the results has been evaluated by calculating % deviations from recommended/literature/certified values.     

Multielement Analysis of South Serbian Strawberry Cultivars by Inductively Coupled Plasma—Optical Emission Spectrometry

The contents of 17 elements in thirteen strawberry cultivars grown in the five districts of Southern Serbia were determined using inductively coupled plasma optical emission spectrometry (ICP-OES). The most abundant elements are K (875–1148 mg?·?kg^?1 fresh weight), P (307–664 mg?·?kg^?1 fresh weight), Ca (192–256 mg?·?kg^?1 fresh weight), and Mg (111–189 mg?·?kg^?1 fresh weight) in all samples. Strawberries were also found to be a good source of Sr (8.05–18.6 mg?·?kg^?1 fresh weight) and Fe (3.09–10.4 mg?·?kg^?1 fresh weight). The contents of As and Cd were below the detection limit (0.0828 mg?·?kg^?1 and 0.0205 mg?·?kg^?1, respectively) in all strawberry samples, while the contents of Ni, Cr, and Cu were below the recommended tolerable levels proposed by Joint Food and Agriculture Organization of the United Nations and World Health Organization Expert Committee on Food Additives, and did not a pose a health risk for the consumer. The application of Duncan’s test showed significant differences between contents of analyzed elements in all strawberry cultivars. The highest mean levels of analyzed elements were detected in strawberries grown in the Topli?ki, Jablani?ki, and P?injski districts. The spike recovery test was used to verify the accuracy of the method, and the spike recovery was in the range 93.8–107.8%. The contents of the metals in strawberry samples were also comparable with values previously reported in the literature.     

Development of a certified reference material for the determination of acrylamide in potato chips

A certified reference material (CRM), KRISS CRM 108-10-003, has been developed for analysis of acrylamide in potato chips, as a representative of carbohydrate-rich food cooked in high-temperature oil. The material was prepared by grinding commercially available potato chips to a paste which was then homogenized, bottled in 15-g units, and stored at ?70 °C. Certification, homogeneity and stability testing, were carried out by liquid chromatography–isotope-dilution mass spectrometry (ID-LC–MS). A single ID-LC–MS measurement was performed for each of 10 selected units for certification and homogeneity assessment. The mean measurement result for the 10 bottles, 0.455?±?0.012 mg?kg^?1, was assigned as the certified value of the CRM. The between-bottle homogeneity was 0.8% of the certified value. The within-bottle homogeneity, tested by measuring three replicate sub-samples from each of three randomly selected bottles, was similar to the between-bottle homogeneity. The stability of the CRM under storage conditions (?70 °C) was tested for 21 months and no change in the acrylamide content was observed within the measurement uncertainty. Stability of the CRM at –20 °C (storage at user’s site) and room temperature (for regular use and transportation) was also tested. Also presented is the newly designed procedure for evaluating the uncertainty of the certified value for the characterization scheme used in this study.

Development of a certified reference material for the determination of perfluorooctanoic acid

A certified reference material (CRM) for the determination of perfluorooctanoic acid (PFOA) has been issued as NMIJ CRM 4056-a by the National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Purity (kg kg^?1) based on a titration method was determined by subtracting the mass fractions of impurities measured using liquid chromatography/mass spectrometry (LC/MS) from those of acids expressed as PFOA measured by a neutralization potentiometric titration. To validate an obtained result, purity based on a mass balance method was determined by subtracting the mass fractions of impurities, measured using LC/MS, Karl-Fischer titration (KFT), and vacuum evaporation, from 1 kg kg^?1. Results from both titration and mass balance methods were in agreement within the accepted limits of uncertainty. The certified purity of NMIJ CRM 4056-a was determined to be 0.959 kg kg^?1, calculated as the mean of the results obtained with the two methods. The standard uncertainty of the certified purity was evaluated from purity evaluations as well as from sample homogeneity and stability obtained from LC/MS and KFT analyses. Consequently, the expanded uncertainty was estimated to be 0.005 kg kg^?1 with a coverage factor of k = 2.     

Certified calibration solution reference material for the determination of perfluorooctane sulfonate from the National Metrology Institute of Japan (NMIJ)

A new calibration solution reference material for the determination of perfluorooctane sulfonate anion (PFOS) and its salts has been issued as a certified reference material (CRM) by the National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). The purity amount-of-substance fraction of raw material potassium perfluorooctane sulfonate (K-PFOS) was evaluated based on the results obtained using the freezing point depression method, and the purity mass fraction of the raw material was calculated using the average molar mass of impurities, the molar mass of K-PFOS, and the purity amount-of-substance fraction. The certified concentration of this CRM was obtained by multiplying the dilution ratio of the raw material in a prepared solution (methanol) determined from the gravimetric blending method by the purity of the raw material. The preparation concentration of K-PFOS as a certified value of NMIJ CRM 4220-a was determined to be 9.93?mg?kg^?1. In addition, the standard uncertainty of the certified value was evaluated from the purity evaluation as well as from sample inhomogeneity, instability, and preparation variation obtained from LC/MS measurements of different gravimetrically prepared solutions of the NMIJ CRM. Consequently, the expanded uncertainty was estimated to be 0.15?mg?kg^?1 with a coverage factor k?=?2 corresponding to the half-width of estimated confidence interval of approximately 95%.     

Characterization of water content in biodiesel fuel certified reference material (NMIJ CRM 8302-a)

The National Metrology Institute of Japan has issued a certified reference material of biodiesel fuel derived from palm oil (NMIJ CRM 8302-a) for the measurement and quality control of water, methanol, six elements (sulfur, phosphorus, sodium, potassium, magnesium, and calcium), density, and kinematic viscosity. This paper presents the technical details for the characterization of the water content in NMIJ CRM 8302-a. Because the water content in biodiesel is easily affected by ambient humidity, sample handling is extremely difficult. Thus, a sample handling technique that overcomes this limitation was established, and optimized coulometric and volumetric Karl Fischer titrations were performed in order to accurately determine the water content with traceability to the International System of Units. The certified water content and its expanded uncertainty with a coverage factor k = 2 were 393 mg kg^?1 and 25 mg kg^?1, respectively.     

GC-MS analysis of the PCB substitute Ugilec 141 and its occurrence in waste mineral oils

After the restrictions on production and use of PCBs, Ugilec 141, a technical mixture of dichlorobenzyldichlorotoluenes (DBDTs), has been used as a PCB substitute in hydraulic systems. In the Netherlands, the production, import and use of Ugilec 141 has been forbidden since 1988. A method has been developed for the analysis of Ugilec 141 in waste mineral oils to control waste oil import and processing. The method development was based on modification of procedures for the analysis of PCBs in oil and dioxins in fatty matrices and analysis was performed with gas chromatography with mass spectrometry. For sample clean-up, several combinations of column chromatography with activated carbon, alumina, and silica gel have been tested to obtain extracts free from matrix interferences. An internal standard of ¹³C-labeled DBDT was examined to check recoveries from the clean-up procedures. Quantification was performed by comparison with the six most abundant peaks of an external Ugilec 141 standard mixture. Validation experiments showed a linear range from 0.25 to 60 mg Ugilec 141 kg^?1 oil, a reproducibility of 3% and a limit of determination of 0.25 mg Ugilec 141 kg^?1 waste oil. The method was applied in a survey of 70 samples of waste mineral oils from producers all over the Netherlands; this revealed levels below the limit of determination and one positive sample with a concentration of 5.7±0.1 mg Ugilec 141 kg^?1 oil. In an inspection inquiry, one contaminated oil was found containing 116 ± 9 g Ugilec 141 kg^?1 oil.     

Pesticide residue levels in peppers cultivated in Souss Masa valley (Morocco) after multiple applications of azoxystrobin and chlorothalonil

Residue levels of azoxystrobin and chlorothalonil were determined in peppers grown in an experimental greenhouse. These two pesticides were selected on the basis of previous excesses of 26 and 24%, respectively, found in peppers samples cultivated in 2008 in eastern Morocco. The measurements were made over a 7 week period in which up to three successive treatments with azoxystrobin and a 4 week period in which up to three successive treatments with chlorothalonil were carried out. In all cases, plants were sprayed separately with azoxystrobin and chlorothalonil with application rates of active ingredients of 50 and 200?cc?hl^?1, respectively. Sampling was carried out at 0, 2, 4, 7, 12, 15 and 22 days for azoxystrobin and 0, 1, 3, 7, 8 and 10 days for chlorothalonil. Residue levels of azoxystrobin and chlorothalonil were determined by liquid–liquid extraction (LLE) and gas chromatography with electron-capture detector (GC-ECD). During the study, residue levels in the plantation ranged between 1.14 and 0.02?mg?kg^?1 for azoxystrobin and between 0.55 and 0.04?mg?kg^?1 for chlorothalonil. The application of an intensive washing process to the pepper samples did not lead to a significant reduction in the residue levels of either pesticide. Likewise, significant differences were not found between the residue levels in the ‘edible’ and ‘inedible’ parts of the peppers.     

Determination of rare earth elements in Indian kimberlite using inductively coupled plasma mass spectrometer (ICP-MS)

A method has been developed for the analysis of rare earth elements (REEs) in kimberlite samples using inductively coupled plasma mass spectrometer (ICP-MS). The samples were dissolved using sodium peroxide fusion and after appropriate dilutions the solutions were analyzed using ICP-MS. The paper presents the concentration of rare-earth elements as determined by ICP-MS in eight kimberlite samples from Central India. The method was validated using certified reference materials STSD-1 and STSD-2 from Canadian Certified Reference Material Project. The method detection limit of various REEs varies from 0.12 to 1.54?mg?kg^?1. The total REE concentrations range from 418 to 726?mg?kg^?1 and fall within the interval of those reported in the literature for kimberlites. Despite the marked difference in the REE contents, all the analyzed samples show similar REE patterns that resemble those for kimberlites. In order to compare ICP-MS results, the samples were analyzed using instrumental neutron activation analysis which is a reference method for determination of REEs in geological samples.     

Determination of cadmium and lead in plastic material from waste electronic equipment using solid sampling graphite furnace atomic absorption spectrometry

The European initiatives to minimize waste electric and electronic equipment (WEEE) and the restriction of hazardous substances (RoHS) had a major impact on the routine control of hazardous substances, including toxic trace metals, such as cadmium and lead, in all kinds of materials that are used in electric and electronic equipment. Instead of analyzing a whole computer, cell phone or television set, individual parts are normally investigated in order to simplify the analytical task. Plastic components are important constituents of electronic equipment, and a potential source of toxic trace metals that are added as catalysts, stabilizers or colorants. As high-tech plastic materials are designed to be resistant against chemical attack, they are usually difficult to bring into solution. A procedure is proposed in the present work that uses direct solid sampling graphite furnace atomic absorption spectrometry and calibration against aqueous standards. The method is sensitive, fast, and it does not require any sample preparation. The limits of detection of 0.1 mg kg^− 1 for Cd and 0.6 mg kg^− 1 for Pb are more than adequate for the purpose. Additional means are presented for reducing the sensitivity in order to cope with high analyte concentration. The method has been tested analyzing two certified reference materials, and good agreement with certified values has been obtained.     

Development and certification of a reference material for Fusarium mycotoxins in wheat flour

Deoxynivalenol (DON), nivalenol (NIV) and zearalenone (ZEN) are toxic secondary metabolites produced by several species of Fusarium fungi. These mycotoxins are often found together in a large variety of cereal-based foods, which are regulated by maximum content levels of DON and ZEN. To date, suitable certified reference materials (CRM) intended for quality control purposes are lacking for these Fusarium mycotoxins. In order to overcome this lack, the first CRM for the determination of DON, NIV and ZEN in naturally contaminated wheat flour (ERM®-BC600) was developed in the framework of a European Reference Materials (ERM®) project. This article describes and discusses the whole process of ERM®-BC600 development, including material preparation, homogeneity and stability studies, and an interlaboratory comparison study for certification. A total of 21 selected expert laboratories from different European countries with documented expertise in the field of mycotoxin analysis took part in the certification study using various gas and liquid chromatographic methods. The certified values and their corresponding expanded uncertainties (k?=?2) were assigned in full compliance with the requirements of ISO Guide 35 and are as follows: 102?±?11 μg?kg^?1 for DON, 1000?±?130 μg?kg^?1 for NIV and 90?±?8 μg?kg^?1 for ZEN.     

Simultaneous determination of Cd,Cr, Cu,Ni, Pb and Zn in sewage sludge by slurry introduction ICP-OES method

In order to evaluate the slurry nebulisation method as an alternative method for analysis of sewage sludge, the metal content of sludge samples of different origins was determined. The concentrations of six elements: Cd, Cr, Cu, Ni, Pb, and Zn were determined by introducing the sludge as a slurry into an inductively coupled plasma optical emission spectrometer (ICP-OES). Calibration was performed by using aqueous standard solutions. For comparison, the sewage sludge was also digested by microwave digestion and introduced into the plasma as an aqueous solution. The accuracy of the method was checked by analysing a sewage sludge certified reference material (CRM 007-040 Sewage Sludge). The Student's t-test showed that values obtained using slurry nebulisation were close to the certified values at a 95% confidence level. The values of elements Cd 11.1?±?0.8; Cr 37.7?±?3.3; Cu 563.3?±?38.4; Pb 119.2?±?10.1; Zn 729?±?68.2?mg?kg^?1 obtained using this method were comparable with those obtained using the conventional method. The slurry method can, therefore, be successfully applied to the determination of content of each element in sewage sludge with RSD less than 3%, without the need to predissolve them. This could avoid the use of hazardous chemicals, incomplete dissolution and loss of volatile analytes.     

Study of arsenic (As) mobilization in the Ganga Alluvial Plain using neutron activation analysis

In northern part of Indian sub-continent, As related environmental and health issues receive attention from all over the world. Forty-eight sediment samples were collected from the Ganga Alluvial Plain (GAP) and its weathering products (from the Gomati River) for the study of As distribution and mobilization. These sediment samples were analyzed by Instrumental Neutron Activation Analysis (INAA) method using Cirus Research Reacter of Bhabha Atomic Research Centre, Mumbai. Average As concentrations in the GAP sediments (10.44?mg?kg^?1), the Gomati River bed sediments (1.36?mg?kg^?1) and the Gomati River suspended sediments (5.30?mg?kg^?1) were reported. Significant decrease of As content from the alluvial sediments to the river sediments is a clear indication of its mobilization by chemical weathering processes of mineral biotite. Present study demonstrates the importance of INAA for quantification and mobilization of As and improves our understanding related to As related environmental issues in northern India and elsewhere.     

Adsorption of Cu(II) ions from aqueous solution by hazelnut husk activated carbon prepared with potassium acetate

Hazelnut husk (HH), an agricultural waste, was converted to carbonaceous material by chemical activation using potassium acetate. The produced activated carbon (KAHHAC) was characterized by FTIR, SEM, N₂ adsorption–desorption experiments, CHN elemental analysis, and determination of moisture, ash, and point of zero charge. KAHHAC was used for the batch adsorption of Cu(II) ions from aqueous solutions. Optimum pH and contact time were found to be 5.0 and 240 minutes, respectively. The adsorption equilibrium data were described well by the Langmuir equation providing 105.3?mg?g^?1 Cu(II) adsorption capacity. The pseudo-second-order model successfully described the kinetic of Cu(II) adsorption by KAHHAC. The adsorbed Cu(II) onto KAHHAC was completely desorbed by 0.5?M nitric acid. In conclusion, HH activated carbon (AC) produced by the potassium acetate activation method is a very useful and efficient sorbent material for the removal of Cu(II) from aqueous solution.     

Copper content of vineyard soils at Sremski Karlovci (Vojvodina Province,Serbia) as affected by the use of copper-based fungicides

The present study investigated the copper content of nine vineyard plots soils and four control plots as affected by the application of copper-based fungicides. The study was carried out at the site of Sremski Karlovci in the Serbian province of Vojvodina. The results showed that Cu soil concentrations are increased at the site and that there is a tendency towards soil contamination by this element. Of the 27 total samples studied, only one had Cu concentration above the maximum allowable concentration of 100?mg?kg^?1. That sample's concentration was 111.7?mg?kg^?1. All the samples from the 0–15?cm layer had copper levels that were above the critical value of 60?mg?kg^?1. The mean value of the samples was 79.4?mg?kg^?1, contrasting with the background concentration of 19.8?mg?kg^?1. The results obtained for the studied vineyard soils indicate that these soils are potentially at risk and call for reduced application of Cu-based fungicides along with soil monitoring.     

New methods for acceleration of meat sample preparation prior to determination of the metal content by atomic absorption spectrometry

Focused microwave-assisted digestion and ultrasound leaching have been applied for the extraction of Pb, Cd, Cr, Cu, Fe, Zn, Ca, and Mg from raw meat. Semimembranous muscle (SM) of raw pig ham was used for optimizing both the digestion and extraction steps by multivariate approaches. The detection and quantification limits were 0.5 and 0.9 g kg^–1 for Pb, 0.06 and 0.1 g kg^–1 for Cd, 0.2 and 1.2 g kg^–1 for Cr, 0.4 and 3 g kg^–1 for Cu, 0.04 and 0.1 mg kg^–1 for Fe, 0.012 and 0.017 mg kg^–1 for Zn, 0.3 and 0.4 mg kg^–1 for Ca, and 0.01 and 0.03 mg kg^–1 for Mg. The precision, expressed as relative standard deviation (RSD), ranged between 2.5 and 9.6% for focused microwave-assisted digestion and between 3.5 and 10.6% for ultrasound leaching. The methods were then compared with a reference method and applied to a certified reference material (bovine muscle 184, from the BCR). The t-test, applied to the results obtained from focused microwave-assisted digestion, revealed that they are in agreement (p>0.01) with the certified and estimated values in the case of Pb, Cd, Cr, Cu, Fe, Ca, Mg, and Zn but not in that of Fe. In the case of ultrasound leaching, only the extraction of Pb, Cu, and Ca was quantitative. The method based on microwave digestion provides more accurate and precise results than ultrasound leaching. These new procedures have many advantages with regards to conventional methods, namely, reduction of the extraction time, simplification of the process, avoidance of chemical emissions to the atmosphere, and no losses of metals by volatilization.     

Certification of the mass fractions of trace elements and pentachlorophenol in an impregnated wood reference material

The resource-saving utilisation of recovered waste wood is a matter of growing concern. In several European countries, this utilisation is governed by regulations and is dependent on the contents of certain trace elements and organic compounds. Thus, for decision-making with respect to waste wood management (recycling or combustion), reliable analytical data are needed and, due to their great economic and environmental impact, must be assured by appropriate quality control. To support the improvement in quality assurance in waste wood analysis, for the first time, a wood reference material was certified for its mass fractions of arsenic, cadmium, chromium, copper, lead, mercury, and pentachlorophenol (PCP). These analytes were selected because they represent typical constituents of wood preservatives most widely used in the past. Material preparation and testing of homogeneity and stability were carried out by BAM Federal Institute for Materials Research and Testing. The certification measurements were performed involving selected laboratories with documented expertise in the field of waste wood analysis. The certified values and their corresponding uncertainties were assigned in full compliance with the requirements of ISO Guide 35. The certified mass fractions and their expanded uncertainties (k = 2) are as follows: (3.1 ± 0.5) mg/kg for As, (3.02 ± 0.24) mg/kg for Cd, (36.4 ± 2.6) mg/kg for Cr, (22.9 ± 1.7) mg/kg for Cu, (0.60 ± 0.14) mg/kg for Hg, (39 ± 4) mg/kg for Pb, and (7.9 ± 0.6) mg/kg for PCP. The certified material is available as European Reference Material ERM^®-CD100.     

Dissipation of insect growth regulators in fresh and canned fruits

The objective of the study was to determine the dissipation of insect growth regulators in fresh and canned mandarin and apricot to determine the exposure to them. Field studies were carried out in the preharvest period with good agricultural practices (GAP) and in critical agricultural practices. The processing studies were carried out in each relevant step in a pilot plant. A validated methodology was developed (limit of quantification of 0.05?mg?kg^?1 for apricots, 0.10?mg?kg^?1 for mandarin) including acetone–dichloromethane extraction, cleanup, and liquid chromatography-diode array detection. The pesticides complied with the maximum residue limits (MRLs) except pyriproxyfen, which has not been authorized in apricots, and it did not comply with its MRL for peaches. The dissipation rates (t _1/2) with GAP were fenoxycarb-apricot?>?pyriproxyfen-apricot?>?fenoxycarb-mandarin?>?pyriproxyfen-mandarin. In the processing studies, there was only residue transference in the canning of apricots. All final cans contained residues much lower than the MRLs.     

Determination of zinc in marine/lacustrine sediments by graphite furnace atomic absorption spectrometry using Pd/Mg chemical modifier and slurry sampling

Effectiveness of Pd/Mg chemical modifier for the accurate direct determination of zinc in marine/lacustrine sediments by graphite furnace atomic absorption spectrometry (GF-AAS) using slurry samples was evaluated. A calibration curve prepared by aqueous zinc standard solution with addition of Pd/Mg chemical modifier is used to determine the zinc concentration in the sediment. The accuracy of the proposed method was confirmed using Certified Reference Materials, NMIJ CRM 7303-a (lacustrine sediment) from National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology, Japan, and MESS-3 (marine sediment) and PACS-2 (marine sediment) from National Research Council, Canada. The analytical results obtained by employing Pd/Mg modifier are in good agreement with the certified values of all the reference sediment materials. Although for NRC MESS-3 an accurate determination of zinc is achieved even without the chemical modifier, the use of Pd/Mg chemical modifier is recommended as it leads to establishment of a reliable and accurate direct analytical method. One quantitative analysis takes less than 15 minutes after we obtain dried sediment samples, which is several tens of times faster than conventional analytical methods using acid digested sample solutions. The detection limits are 0.13?µg?g^?1 (213.9?nm) and 16?µg?g^?1 (307.6?nm), respectively, in sediment samples, when 40?mg of dried powdered samples are suspended in 20?mL of 0.1?mol?L^?1 nitric acid and a 10?µl portion of the slurry sample is measured. The precision of the proposed method is 8–15% (RSD).