Simultaneous oxidation and removal of Sb(III) from water by using synthesized CTAB/MnFe2O4/MnO2 composite.

Low levels of antimony (Sb) can be effectively removed from water by adsorption onto various materials, and searching for low-cost and high-efficiency new adsorbents has been a hot topic in recent years. In the present study, the performance of cetyltrimethylammonium bromide (CTAB) modified MnFe2O4/MnO2 composites (CTAB/MnFe2O4/MnO2) as an adsorbent for Sb(III) removal from aqueous solution was investigated. Kinetic study revealed that adsorption of Sb(III) by CTAB/MnFe2O4/MnO2 was fast in the first 430 min and the equilibrium was achieved within 1440 min. The adsorption kinetic data were well fitted with pseudo-second-order model. The maximum adsorption capacity of the synthesized adsorbent for Sb(III) at pH 7 calculated from Langmuir adsorption isotherms in batch experiments was 321.03 mg g-1. During the adsorption process, Sb(III) can be simultaneously oxidized to Sb(V) and the average oxidation percentage reached 95.43% within 1440 min. The adsorption capacity did not significantly vary with pH. Common metal cations (Ca2+ and Mg2+) slightly enhanced Sb(III) adsorption at pH 7. In comparison, the effect of anions (Cl-, NO3-, and PO43-) on Sb(III) adsorption was not obvious. The results suggest that CTAB/MnFe2O4/MnO2 is a potential cost-effective adsorbent for Sb(III) removal in water treatment.

A simple, rapid and green ultrasound assisted and ionic liquid dispersive microextraction procedure for the determination of tin in foods employing ETAAS.

This paper proposes a simple, rapid and green ultrasound assisted and ionic liquid dispersive microextraction procedure using pyrocatechol violet (PV) as complexing reagent and 1-hexyl-3-methylimidazolium bis(trifluoromethylsulfonyl)-imide [C6MIM][Tf2N] as ionic liquid for the detection of tin employing electrothermal atomic absorption spectrometry (ETAAS). The optimization step was performed using a two-level full factorial design involving the following factors: pH of the working media, amount reagents, ionic liquid volume and extraction time and the chemometric response was tin recovery. The procedure allowed the determination of tin with limits of detection and quantification of 3.4 and 11.3 ng L-1, respectively. The relative standard deviation was 4.5% for a tin solution of 0.50 µg L-1. The validation method was confirmed by analysis of rice flour certified reference material. The method was applied for the quantification of tin in several food samples. The concentration range found varied from 0.10 to 1.50 µg g-1.

Preconcentration of Sn (II) using the methylene blue on the activated carbon and its determination by spectrophotometry method.

A simple and accurate spectrophotometric method for determination of trace amounts of Sn (II) ion in soil sample was developed by using the methylene blue (MB) in the presence of activated carbon (AC) as the adsorbent Solid Phase Extraction (SPE) of Sn (II) and then determined by UV-Vis. The Beer's law is obeyed over the concentration range of 1-80ngmL(-1) of Sn (II) with the detection limits of 0.34ngmL(-1). The influence of type and volume of eluent, concentration of MB, pH, and amount of AC on sensitivity of spectrophotometric method were optimized. The method has been successfully applied for Sn (II) ion determination in soil sample.

Quantification of toxic metals derived from macroplastic litter on Ookushi Beach, Japan.

The potential risk of toxic metals that could leach into a beach environment from plastic litter washed ashore on Ookushi Beach, Goto Islands, Japan was estimated by balloon aerial photography, in situ beach surveys, and leaching experiments in conjunction with a Fickian diffusion model analysis. Chromium (Cr), cadmium (Cd), tin (Sn), antimony (Sb), and lead (Pb) were detected in plastic litter collected during the beach surveys. Polyvinyl chloride (PVC) fishing floats contained the highest quantity of Pb. Balloon aerial photography in conjunction with a beach survey gave an estimated mass of Pb derived from plastic litter of 313 ± 247 g. Lead leaching experiments on collected PVC floats showed that Pb in the plastic litter could leach into surrounding water on the actual beach, and that plastic litter may act as a "transport vector" of toxic metals to the beach environment. Using the experimental data, the total mass of Pb that could leach from PVC plastic litter over a year onto Ookushi Beach was estimated as 0.6 ± 0.6 g/year, suggesting that toxic metals derived from plastic beach litter are a potential "pathway" to contamination of the beach environment due to their accumulation in beach soil over time.

Leaching studies for tin recovery from waste e-scrap.

Printed circuit boards (PCBs) are the most essential components of all electrical and electronic equipments, which contain noteworthy quantity of metals, some of which are toxic to life and all of which are valuable resources. Therefore, recycling of PCBs is necessary for the safe disposal/utilization of these metals. Present paper is a part of developing Indo-Korean recycling technique consists of organic swelling pre-treatment technique for the liberation of thin layer of metallic sheet and the treatment of epoxy resin to remove/recover toxic soldering material. To optimize the parameters required for recovery of tin from waste PCBs, initially the bench scale studies were carried out using fresh solder (containing 52.6% Sn and 47.3% Pb) varying the acid concentration, temperature, mixing time and pulp density. The experimental data indicate that 95.79% of tin was leached out from solder material using 5.5M HCl at fixed pulp density 50 g/L and temperature 90°C in mixing time 165 min. Kinetic studies followed the chemical reaction controlled dense constant size cylindrical particles with activation energy of 117.68 kJ/mol. However, 97.79% of tin was found to be leached out from solder materials of liberated swelled epoxy resin using 4.5M HCl at 90°C, mixing time 60 min and pulp density 50 g/L. From the leach liquor of solder materials of epoxy resin, the precipitate of sodium stannate as value added product was obtained at pH 1.9. The Pb from the leach residue was removed by using 0.1M nitric acid at 90°C in mixing time 45 min and pulp density 10g/L. The metal free epoxy resin could be disposed-of safely/used as filling material without affecting the environment.

Hydrometallurgical treatment of used printed circuit boards after thermal treatment.

The hydrometallurgical route of copper and tin extraction from printed circuit boards (PCB) of used personal computers after thermal pretreatment is discussed. The PCB fractions crushed and sorted into -8+0, -8+3 and -3+0 mm were used for the experiments. The samples were thermally pretreated at temperatures of 300, 500, 700 and 900 °C during 15, 30 and 60 min with the presence of air (burning) before the leaching process. The leaching solution of 1M HCl and temperature of 80 °C was used for the leaching. The original as well as thermally pretreated samples were leached under these conditions. The weight losses within the range from 5% to 35% were achieved by burning depending on the burning temperature. The increase of burning temperature causes the copper extraction into solution up to 98%, while copper extraction into solution from non-burned samples was up to 6%. The opposite effect was observed in the case of the tin leaching, where the highest extraction was achieved when the original sample was leached. The increase of the burning temperature caused the lowering of the copper extraction.

Processing of spent platinum-based catalysts via fusion with potassium hydrogenosulfate.

This work describes a route for processing spent platinum-based commercial catalysts (Pt and PtSnIn/Al(2)O(3)) via fusion with potassium hydrogenosulfate (KHSO(4)). Samples were previously ground. The optimized experimental parameters were: temperature, 450°C; time, 3h; sample/flux mass ratio, 1/10. The fused mass was dissolved in water and the elements present were isolated by a multi-step separation procedure. Platinum was recovered as the only water-insoluble residue. About 45 wt% of aluminium was recovered as KAl(SO(4))(2)·12H(2)O (alum), whereas the remaining element was recovered as Al(OH)(3). Tin and indium were recovered together as sulfides at pH 1. About 72 wt% of potassium was recovered as K(2)SO(4) when the final effluent was treated with sulfuric acid (pH 1) and slowly evaporated. Generation of final wastes was greatly reduced. More than 98 wt% of the elements present in the catalysts examined was recovered.

Leaching of copper and tin from used printed circuit boards after thermal treatment.

The hydrometallurgical route of copper and tin extraction from printed circuit boards (PCBs) of used personal computers after thermal pretreatment is discussed. The samples were thermally pretreated within temperature range of 300-900°C during 15, 30 and 60 min. Two methods of the thermal pretreatment were studied: burning and pyrolysis. The leaching solution of 1 M HCl at 80°C was used. The original as well as thermally pretreated samples were leached. The weight losses within the range from 5 to 35% were achieved. The increase of burning temperature causes the copper extraction into solution up to 98%, while copper extraction into solution from non-burned samples was up to 6%. In the case of the tin leaching the highest extraction was achieved when the original sample was leached. The increase of the burning temperature caused the lowering of the copper extraction. The increase of the pyrolysis temperature enhances copper and tin extraction.

Accelerated solvent-based extraction and enrichment of selected plasticisers and 4-nonylphenol, and extraction of tin from organotin sources in sediments, sludges and leachate soils.

Enrichment techniques have become an important feature in the trace analysis of oestrogen mimicking chemicals in the environment. Recent developments such as accelerated solvent extraction (ASE) have improved extraction recoveries in a wide variety of solid matrices including sediments, sludges and leachate soils. Such samples taken from the Irish Midlands Shannon Catchment region during the winter of 2004/5 and suspected to contain certain xenooestrogens or hormonally active agents were extracted using this technique, which was then coupled with high performance liquid chromatography (HPLC) for quantification purposes. ASE was thus employed to both isolate and pre-concentrate targeted analytes using the minimum amount of solvent hence making extractions more conservational. Two simple, yet extremely sensitive liquid chromatographic methods were developed based on UV detection; one for phthalates and one for alkylphenols, with recoveries reaching up to 92.0%. Acid digestion was used for the extraction of the tin and organotin compounds with analysis by polarography. In river sediment, levels of up to 24.4 mg kg(-1) phthalate, 1.14 mg kg(-1) 4-nonylphenol and 118 mg kg(-1) tin were found. In leachate sediments, values up to 49.8 mg kg(-1) phthalate, 1.57 mg kg(-1) 4-nonylphenol, and 36.0 mg kg(-1) tin were determined. In sludge, values up to 174 mg kg(-1) phthalate and 22.8 mg kg(-1) 4-nonylphenol were quantified. The highest value of tin (118 mg kg(-1)) was found present in an area of high leisure craft activity. Typical sediment levels of tin at other river locations ranged between 1.20 and 37.5 mg kg(-1).

Mass-independent isotopic fractionation of tin in chemical exchange reaction using a crown ether.

Tin isotopes were fractionated by the liquid-liquid extraction technique with a crown ether, dicyclohexano-18-crown-6. The isotopic ratios of (m)Sn/(120)Sn (m: 116, 117, 118, 119, 122 and 124) were measured by multi-collector inductively coupled plasma spectrometry (MC-ICP-MS) on a Nu Plasma 500 with a precision better than 0.05 permil amicro(-1) on each isotopic ratio. Odd atomic mass isotopes ((117)Sn and (119)Sn) showed depletions compared to the even atomic mass isotopes ((116)Sn, (118)Sn, (122)Sn and (124)Sn). We show that this odd-even staggering property originates from the nuclear field shift effect. The contribution of the nuclear field shift effect to the observed isotope enrichment factor was estimated to be approximately 35%.

Simultaneous co-extraction of organometallic species of different elements by accelerated solvent extraction and analysis by inductively coupled plasma mass spectrometry coupled to liquid and gas chromatography.

This paper describes the development of an accelerated solvent extraction methodology that is capable of simultaneously extracting organometallic species of As, Sn and Hg in a semi-automated manner. Accelerated solvent extraction (ASE) methods based on previous research on the separate extraction of organotin and -arsenic species in our laboratory were adapted for the co-extraction of six different species from an oyster tissue certified reference material (BCR 710). For the first time, the extraction of MeHg by this technique is also investigated. The proposed ASE conditions employed 50% acetic acid in methanol at a temperature of 100 degrees C with up to five consecutive extraction cycles of 3 minutes. Extraction efficiencies for organoarsenic species ranged from 80% (dimethylarsinic acid, DMA) to 99% for arsenobetaine (AsB). Species of toxicological interest, such as dibutyltin (DBT), tributyltin (TBT) and methylmercury (MeHg), were extracted with mean recoveries of 81, 84 and 76%, respectively. The extracted species were analysed by gas chromatography/inductively coupled plasma mass spectrometry (GC/ICPMS; DBT, TBT and MeHg) and liquid chromatography/inductively coupled plasma mass spectrometry (LC/ICPMS; MMA, DMA, AsB) after ethylation with sodium tetraethylborate or dilution with water, respectively. In addition to those species for which the extraction efficiency was assessed during this study, a further five arsenic species (arsenite, arsenate and three unidentified species), as well as monobutyltin (MBT) and mono-, di- and triphenyltin, could also be extracted from other matrices. The developed ASE method provides a significant improvement over many currently available routine monitoring methods for trace element speciation due to the fact that it is capable of extracting several species of toxicological interest simultaneously and quantitatively.

Application of experimental design in a method for screening sediments for global determination of organic tin by electrothermal atomic absorption spectrometry (ETAAS).

An experimental design was developed to obtain a simple procedure for global determination of organic tin compounds in sediment. Sediment was extracted by a two-phase method and tin was determined in the organic extract by electrothermal atomic absorption spectrometry (ETAAS), with palladium as chemical modifier. A Plackett-Burman design for screening and a fractional central composite design (CCD) for optimizing were used for evaluation of the effects of several variables. The results showed that sediment mass, volume and concentration of extracting acid, pyrolysis and atomization temperatures, and modifier concentration affect the determination. Reference material PACS-2 was analyzed to evaluate the procedure. It was possible to extract 82% of the organotin content certified in the reference sediment. The limit of detection (LOD) was 0.08 microg g(-1) and the relative standard deviation was 4%. The method was applied to the analysis of estuarine superficial sediments from Gipuzkoa (Spain). The organotin content of these samples ranged from 0.7 to 7.7 microg g(-1), as tin, on a dry-weight basis.

Element selective detection for supercritical-fluid chromatography.

This manuscript describes the use of Supercritical-Fluid Chromatography (SFC) with plasma spectrometric detection for the analysis of organometallics. An introduction on the principles and characteristics of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) is included, along with a discussion about requirements for coupling SFC to plasma detection and the different approaches for interfacing SFC to ICP. The last part of this review paper provides a comprehensive description of SFC-ICP applications for the analysis of organometallics containing iron, silicon, tin, chromium, arsenic, lead, mercury and antimony.

Separation of metal chelates and organometallic compounds by SFC and SFE/GC.

Supercritical fluid chromatography (SFC) combines the high diffusion coefficients of gas chromatography (GC) and the solubility properties of liquid chromatography (LC). SFC generally requires lower temperatures for chromatographic separations and thus is more suitable for analyzing thermally labile compounds including a number of metal chelates and organometallic compounds. SFC also allows interfacing between supercritical fluid extraction (SFE) and chromatographic analysis of metal-containing compounds. A large number of metal chelates and organometallic compounds can be separated by SFC. This article summarizes SFC separation of various chelates of transition metals, heavy metals, lanthanides and actinides as well as organometallic compounds of lead, mercury, and tin reported in the recent literature. This article also discusses SFC detection systems and the determination of solubility of organometallic compounds by SFC.

[A method of choosing the extractant for the recovery of tin from the internal organs of a human cadaver]. / Metodika vybora ékstragenta dlia izvlecheniia olova iz vnutrennikh organov trupa cheloveka.

The analysis of naphthenic acid revealed that they may be used for tin detection in the cadaveric material due to their high complex-forming ability. Method of extraction-atomic absorption tin determination in human organs was developed on the basis of naphthenic acid use. Modified method which differs from the common one by higher sensitivity and selectivity is presented.

Technical problems associated with the production of technetium Tc 99m tin(II) pyrophosphate kits.

The amount of tin(II) required for adequate reduction, complexation, and stability of technetium Tc 99m pertechnetate in radiopharmaceutical kits, and methods of preventing the loss of tin(II) during formulation of these lyophilized kits are investigated. Tin(II) loss from stannous chloride solutions was studied under several conditions, including room air versus nitrogen atmospheres, during vial filling in a laminar-flow hood with samples frozen on dry ice versus samples at room temperature, during lyophilization, and during storage under refrigerated, ambient, and elevated temperatures. Various amounts of stannous chloride, ranging from 5 to 1000 microgram/ml, were used in formulating sodium pertechnetate Tc 99m kits containing 100 mCi technetium Tc 99m and 0.4 microgram total technetium. Samples were removed at various times; hydrolyzed technetium, pertechnetate, and technetium Tc 99m pyrophosphate were isolated on instant thin-layer chromatography-silica gel and quantified with a scintillation counter. The time necessary to deoxygenate distilled water by nitrogen purging was measured. Several sources of stannous chloride were assayed for tin(II) content. Tin(II) loss occurs rapidly in solution (15% in one hour) unless continuously protected with nitrogen, and during vial filling in a laminar-flow hood unless frozen with dry ice. No substantial loss of tin(II) was detected during lyophilization or during storage of lyophilized product at any of the three temperatures. A minimum of 400 microgram tin(II) was required to provide 90% technetium Tc 99m pyrophosphate at six hours after preparation. Adequate deoxygenation of small quantities (450 ml) of water was accomplished in less than one hour. Some stannous chloride salts were highly oxidized in the dry state, and only high-purity elemental tin wire gave acceptable yields of tin(II).

Toxicologic studies of tin needles at the intrathoracic site of mice.

Male Marsh mice which received a single intrathoracic injection of 4 mg of tin needles at 3 months of age were compared with controls given isotonic saline. The form and size of most of the tin needles were similar to those of asbestos needles which produced mesotheliomas and lung neoplasms in rodents. Water and food intake was markedly reduced for 24 hrs after the injection of tin. Survival rates (followed for 19 months), pathology of the bladder, liver, and kidney, as well as local and general cancer development were not adversely associated with the tin treatment as compared with the tin treatment as compared with controls. The local reaction to the tin included giant cell phagocytosis, nodular fibroplasia, and capillary formation. The failure of the tin needles to induce local neoplasms may relate to their high density as compared with silicates and/or their lack of the unique potential of the silicate particles to stimulate avascular fibrosis.