Single analysis of human hair for determining halogens and sulfur after sample preparation based on combustion reaction.

A single analysis of hair for determining halogens (chlorine, bromine, fluorine, and iodine) and sulfur by ion chromatography with suppressed conductivity and mass spectrometry detection (IC-MS) was proposed. Inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS) were also used to compare the results. For this purpose, 300 mg of human hair were digested by microwave-induced combustion (MIC) using 20 bar of oxygen pressure. The analytes were absorbed in 100 mmol L-1 NH4OH. Trueness of the proposed method was evaluated by analysis of a CRM of human hair; by recovery tests, using standard solution at two levels (50% and 100%), and by comparison of results with those obtained by ICP OES (Cl and S) and ICP-MS (Br and I). Suitable recoveries (ranging from 92 to 105%) were obtained, and the results from CRM analysis did not differ significantly from those described in the certificate. Moreover, results obtained by IC-MS did not present significant differences (p > 0.05) from those obtained by ICP OES and by ICP-MS. Precision was evaluated in terms of repeatability and intermediate precision, and the relative standard deviations were always lower than 8%. The proposed method presented good accuracy and it is a reliable strategy for human hair analysis. Final digests obtained using the MIC method were fully compatible with all proposed determination techniques. Compared to others reported in the literature, the proposed method presents several advantages, especially given that it is possible to determine halogens and sulfur in a single analysis. Graphical abstract.

Determination of trace sulfur in biodiesel and diesel standard reference materials by isotope dilution sector field inductively coupled plasma mass spectrometry.

A method is described for quantification of sulfur at low concentrations on the order of mgkg(-1) in biodiesel and diesel fuels using isotope dilution and sector field inductively coupled plasma mass spectrometry (ID-SF-ICP-MS). Closed vessel microwave-assisted digestion was employed using a diluted nitric acid and hydrogen peroxide decomposition medium to reduce sample dilution volumes. Medium resolution mode was employed to eliminate isobaric interferences at (32)S and (34)S related to polyatomic phosphorus and oxygen species, and sulfur hydride species. The method outlined yielded respective limits of detection (LOD) and limits of quantification (LOQ) of 0.7 mg kg(-1) S and 2.5 mg kg(-1) S (in the sample). The LOD was constrained by instrument background counts at (32)S but was sufficient to facilitate value assignment of total S mass fraction in NIST SRM 2723b Sulfur in Diesel Fuel Oil at 9.06±0.13 mg kg(-1). No statistically significant difference at a 95% confidence level was observed between the measured and certified values for certified reference materials NIST SRM 2773 B100 Biodiesel (Animal-Based), CENAM DRM 272b and NIST SRM 2723a Sulfur in Diesel Fuel Oil, validating method accuracy.

Multivariate optimization of an analytical method for the analysis of dog and cat foods by ICP OES.

Experimental design methodology was used to optimize an analytical method for determination of the mineral element composition (Al, Ca, Cd, Cr, Cu, Ba, Fe, K, Mg, Mn, P, S, Sr and Zn) of dog and cat foods. Two-level full factorial design was applied to define the optimal proportions of the reagents used for microwave-assisted sample digestion (2.0 mol L(-1) HNO3 and 6% m/v H2O2). A three-level factorial design for two variables was used to optimize the operational conditions of the inductively coupled plasma optical emission spectrometer, employed for analysis of the extracts. A radiofrequency power of 1.2 kW and a nebulizer argon flow of 1.0 L min(-1) were selected. The limits of quantification (LOQ) were between 0.03 µg g(-1) (Cr, 267.716 nm) and 87 µg g(-1) (Ca, 373.690 nm). The trueness of the optimized method was evaluated by analysis of five certified reference materials (CRMs): wheat flour (NIST 1567a), bovine liver (NIST 1577), peach leaves (NIST 1547), oyster tissue (NIST 1566b), and fish protein (DORM-3). The recovery values obtained for the CRMs were between 80 ± 4% (Cr) and 117 ± 5% (Cd), with relative standard deviations (RSDs) better than 5%, demonstrating that the proposed method offered good trueness and precision. Ten samples of pet food (five each of cat and dog food) were acquired at supermarkets in Aracaju city (Sergipe State, Brazil). Concentrations in the dog food ranged between 7.1 mg kg(-1) (Ba) and 2.7 g kg(-1) (Ca), while for cat food the values were between 3.7 mg kg(-1) (Ba) and 3.0 g kg(-1) (Ca). The concentrations of Ca, K, Mg, P, Cu, Fe, Mn, and Zn in the food were compared with the guidelines of the United States' Association of American Feed Control Officials (AAFCO) and the Brazilian Ministry of Agriculture, Livestock, and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento-MAPA).

Public health, climate, and economic impacts of desulfurizing jet fuel.

In jurisdictions including the US and the EU ground transportation and marine fuels have recently been required to contain lower concentrations of sulfur, which has resulted in reduced atmospheric SO(x) emissions. In contrast, the maximum sulfur content of aviation fuel has remained unchanged at 3000 ppm (although sulfur levels average 600 ppm in practice). We assess the costs and benefits of a potential ultra-low sulfur (15 ppm) jet fuel standard ("ULSJ"). We estimate that global implementation of ULSJ will cost US$1-4bn per year and prevent 900-4000 air quality-related premature mortalities per year. Radiative forcing associated with reduction in atmospheric sulfate, nitrate, and ammonium loading is estimated at +3.4 mW/m(2) (equivalent to about 1/10th of the warming due to CO(2) emissions from aviation) and ULSJ increases life cycle CO(2) emissions by approximately 2%. The public health benefits are dominated by the reduction in cruise SO(x) emissions, so a key uncertainty is the atmospheric modeling of vertical transport of pollution from cruise altitudes to the ground. Comparisons of modeled and measured vertical profiles of CO, PAN, O(3), and (7)Be indicate that this uncertainty is low relative to uncertainties regarding the value of statistical life and the toxicity of fine particulate matter.

Anti-leishmanial activity of plant-derived acridones, flavaglines, and sulfur-containing amides.

Visceral and cutaneous leishmaniases are an important public health problem in endemic geographic regions in 88 countries worldwide, with around 12 million infected people. Treatment options are limited due to toxicity and teratogenicity of the available drugs, response problems in HIV/Leishmania co-infections, and upcoming resistances. In this study, we investigated the anti-leishmanial activity of 13 plant-derived compounds in vitro aiming to find new drug candidates. Toxicity of the compounds was evaluated in human primary hepatocytes, and hemolytic activity was examined in freshly isolated erythrocytes. Two acridones, 5-hydroxynoracronycine and yukocitrine, two flavaglines, aglafoline and rocaglamide, and the sulfur-containing amide methyldambullin showed promising anti-leishmanial activities with 50% effective concentrations (EC50s) of 34.84, 29.76, 7.45, 16.45, and 6.29 µM, respectively. Hepatotoxic activities of 5-hydroxynoracronycine, yukocitrine, and methyldambullin were significantly lower compared to miltefosine and lower or equal compared to artesunate, whereas the ones of rocaglamide and aglafoline were slightly higher compared to miltefosine and significantly higher compared to artesunate. None of the compounds showed hemolytic activity.

Formation of metacinnabar by milling of liquid mercury and elemental sulfur for long term mercury storage.

In this paper we present the results of the formation of black HgS (metacinnabar) from liquid mercury and elemental sulfur using the mechanical energy provided by a ball mill in different conditions. Metacinnabar formation was observed even after short milling times (15 min) and unreacted liquid mercury was no longer detected after 60 min of milling. The reaction mechanism was monitored with a scanning electron microscope. The impact and friction forces of milling on the Hg and S mixture resulted in the formation of metacinnabar by reducing the size of mercury drops, giving rise to microspheres, and lowering the surface tension to allow sulfur grains to become adhered at the reaction interface. After 60 min of milling, the metacinnabar formation reaction was observed to be more than 99.99% complete, yielding a Toxicity Characteristic Leaching Procedure value of 3.1 microg/L Hg. The reaction product thus complies with the limits of the most stringent Universal Treatment Standard requirements, which allow a maximum TCLP concentration of 25 microg/L.

The effect of federal fuel sulfur regulations on in-use fleets: on-road heavy-duty source apportionment.

From 2002 to 2007 fuel sulfur content in the Minneapolis/St Paul area decreased from about 325 ppm S to <15 ppm S as a result of EPA regulations. We hypothesized that the reduction in fuel sulfur would result in a reduction of fuel specific heavy duty (HD) particle number emissions for the on-road diesel fleet. Fuel specific emissions were estimated by collecting on-road aerosol data, and exploiting the difference in the relative volumes of HD and light duty (LD) traffic on the roadway. Fuel-specific particle number emissions for HD vehicles were measured to be 9.1 +/- 6.6 x 10(15) and 3.2 +/- 2.8 x 10(15) particles/kg of fuel burned, in 2006 and 2007, respectively, a reduction of 65%. In an earlier study in 2002 particle number emissions for the in-use HD fleet were 4.2 +/- 0.6 x 10(15) particles/km compared to the current measurements of 2.8 +/- 2.1 x 10(15) and 9.9 +/- 8.7 x 10(14) particles/km in 2006 and 2007, respectively. The HD particle mass emission standard remained unchanged from 1994 through 2006 and few 2007 HD vehicles were on the road at the time of this study so the decreases in number observed emissions are more likely due to reductions in the sulfur content of the fuel than to changes in engine and aftertreatment design.

A common disinfectant used in condom processing inhibits endonuclease digestion of sperm DNA.

DNA recovered from a condom found at a crime scene appeared undigestible with restriction enzymes, preventing characterization by Southern blot and polymorphic probe hybridization. Several chemical substances used in the processing and treatment of condoms were tested for inhibitory action of restriction enzymes. In particular dibenzalkonium chloride appeared to promote enzyme inhibition at very low concentrations. The effectiveness of treatments to restore cleavage of sample DNA in the presence of such contaminants is discussed.

Determination of radiochemical purity and pharmacokinetic parameters of 99mTc-sulphur colloid and 99mTc-tin colloid.

Labelling yield and radiochemical purity, higher than 95%, of 99mTc-colloid preparations were determined by using the paper chromatography method. Less than 3% of labelled citric acid, added to the preparation as a buffer solution, has been found in 99mTc-sulphur colloid. High radiochemical purity and optimum size of colloid particles has also been proved by biodistribution studies on experimental animals. The analysis performed has shown that more than 50% of 99mTc-colloid preparations excreted by urine is 99mTcO-, the remaining past 50% being protein bound 99mTc. Biological half-time of excretion of the fast phase is the same for both preparations, i.e. 10 min, while for the slow component it is 120 min in 99mTc-S-colloid and 160 min in 99mTc-Sn colloid.