Abstract: Triammonium aurin tricarboxylate (aluminon) has been used to localize aluminum in 2 μm sections of undecalcified, methyl methacrylate embedded bone obtained from patients with terminal chronic renal failure. Aluminum appeared in four cases as bright red lines at the mineralized-bone boundary. In two cases, however, purplish lines were found and one patient showed red as well as purplish lines. Laser microprobe mass analysis (LAMMA) identified aluminum at the location of the red lines and both aluminum and iron at the purplish lines. Furthermore, both iron and aluminum were found in histiocytic bone marrow cells, which showed brownish aluminon staining. It appears that when aluminum and iron occur together, aluminon staining may yield aberrant results. This study shows that LAMMA can be used for the identification of elements sought by histochemical methods and thus permits the evaluation of their staining effects.

Abstract: Ion chromatographic (IC) methods have been compared in order to achieve an optimal separation of fluoride, acetate and formate under various elution conditions on two formerly introduced analytical columns (i and ii) and a novel one (iii): (i) an IonPac AS14 (250 mm × 4 mm I.D.), (ii) Allsep A-2 (150 mm × 4.6 mm I.D.), and (iii) an IC SI-50 4E (250 mm (length) × 4 mm (internal diameter – I.D.)). The IC conditions for the separation of the anions concerned were optimized on the IC SI-50 4E column. A near baseline separation of these anions was attained on the IonPac AS14, whereas the peaks of fluoride and acetate could not be resolved on the Allsep A-2. A baseline separation for the three anions was achieved on the IC SI-50 4E column, when applying an eluent mixture of 3.2 mmol/L Na2CO3 and 1.0 mmol/L NaHCO3 with a flow rate of 1.0 mL/min. The highest precision of 1.7, 3.0 and 2.8% and the best limits of detection (LODs) of 0.014, 0.22 and 0.17 mg/L for fluoride, acetate and formate, respectively, were obtained with the IC SI-50 4E column. Hence, this column was applied for the determination of the acetic and formic acid contents of air samples taken by means of passive gaseous sampling at the Metropolitan Museum of Art in New York, USA. Atmospheric concentrations of acetic and formic acid up to 1050 and 450 μg/m3, respectively, were found in non-aerated showcases of the museum. In galleries and outdoors, rather low levels of acetic and formic acid were detected with average concentrations of 50 and 10 μg/m3, respectively. The LOD data of acetate and formate on the IC SI-50 4E column correspond to around 0.5 μg/m3 for both acetic and formic acid in air samples.

Abstract: Adding 20mg of 1-(2-pyridylazo)-2-naphthol (PAN) to a water sample at 70°, and filtering off the precipitate after cooling, gives efficient preconcentration prior to X-ray fluorescence analysis of water. Up to the capacity of about 100 μeq of PAN used, the trace metal recoveries are around 90% or higher for Cr3+, Mn2+, Ni2+, Cu2+, Zn2+, Hg2+ and Eu3+, and above 70% for many other ions. The recovery yields usually do not vary critically with pH in the neutral pH-range, and are practically independent of the sample salinity, sample volume and trace-metal concentration. Enrichment factors as high as 2 × 105 can be achieved. Counting statistics would then allow detection limits of 0.03 ppM. The blank levels in commercial PAN, however, lead to typical detection limits of about 1 ppm. The coefficient of variation is typically in the 510% range at the 10-ppM level. The accuracy and applicability of the procedure are illustrated by comparative analyses on samples of synthetic solutions, river and drinking water.

Abstract: A novel electrothermal atomic absorption spectrometry (ETAAS) method was developed for the halogenation of refractory sample components (Er, Nd and Nb) of lithium niobate (LiNbO3) and bismuth tellurite (Bi2TeO5) optical single crystals to overcome memory effects and carry-over. For this purpose, the cleaning step of a regular graphite furnace heating program was replaced with a halogenation cycle. In this cycle, after the graphite tube cooled to room temperature, a 20 μL aliquot of liquid carbon tetrachloride (CCl4) was dispensed with a conventional autosampler into the graphite tube. The CCl4 was partially dried at 80 °C under the mini-flow (40 cm3 min−1) condition of the Ar internal furnace gas (IFG), then the residue was decomposed (pyrolyzed) by fast furnace heating at 19002100 °C under interrupted flow of the IFG. This step was followed by a clean-out stage at 2100 °C under the maximum flow of the IFG. The advantage of the present method is that it does not require any alteration to the graphite furnace gas supply system in contrast to most of the formerly introduced halogenation techniques. The effectiveness of the halogenation method was verified with the determination of Er and Nd dopants in the optical crystals. In these analyses, a sensitivity decrease was observed, which was likely due to the enhanced deterioration of the graphite tube surface. Therefore, the application of mathematical correction (resloping) of the calibration was also required. The calibration curves were linear up to 1.5 and 10 μmol L−1 for Er and Nd, respectively. Characteristic masses of 18 and 241 pg and the limit of detection (LOD) values of 0.017 and 0.27 μmol L−1 were found for Er and Nd, respectively. These LOD data correspond to 0.68 μmol mol−1 Er and 11 μmol mol−1 Nd in solid bismuth tellurite samples. The analytical results were compared with those obtained by a conventional ETAAS method and validated with X-ray fluorescence spectrometry analysis.

Abstract: This article reviews the different methods used for the determination of selenium species in all types of environmental waters. Basic difficulties are discussed and the efficiency of the methods is explained in view of the sub-μg/1. concentration levels. Special attention is paid to preconcentration steps. Published data on speciation and concentration levels in various water samples are critically reviewed.

Abstract: Relative sensitivity factors for determination of 41 elements by spark-source mass-spectrometry have been measured. The samples were pressed into graphite electrodes and ionized with a radiofrequency spark. The mass spectra were recorded on a photoplate and the resulting data processed by a computer. Indium was used as standard and the relative sensitivity factors for both singly- and doubly-charged ions were determined with reference to the singly-charged indium ion, with an overall error of 30%. The mean analysis precision was 16%.

Abstract: An investigation was made to determine the influence of the dumping of a 1000 ton day−1, on the average, of acid-iron waste from the titanium dioxide industry into the shallow but turbulent Southern Bight of the North Sea. This waste contains some 20% sulfuric acid and 2% iron. After the passage of the barge that discharges 10 ton of waste min−1 into its wake, the vertical and horizontal distributions of the pH, iron-concentration and turbidity were measured as a function of time. It appeared that a few seconds after the discharge and for a very brief period, the pH was down to approx. 4 and the Fe-concentration was 13 mg l−1. More than 1 min after the discharge a pH below 6 and an iron-level above 3 mg l−1 could not be detected anywhere. The measured factor for waste dilution by sea water, based on the observed acid and iron concentration in the waste and in the discharge track, were around 5000 after 5 min, 9000 after 10 min and 80,000 after 20 min. Before and long after the dumping, the total iron-concentration in this Southern Bight area was around 100 μg l−1, but this high level might be due to natural causes.

Abstract: Many studies probing the link between air quality and health have pointed towards associations between particulate matter (PM) exposure and decreased lung function, aggravation of respiratory diseases like asthma, premature death and increased hospitalisation admissions for the elderly and individuals with cardiopulmonary diseases. Of recent, it is believed that the chemical composition and physical properties of PM may contribute significantly to these adverse health effects. As part of a Belgian Science Policy project (Health effects of particulate matter in relation to physicalchemical characteristics and meteorology), the chemical composition (elemental and ionic compositions) and physical properties (PM mass concentrations) of PM were investigated, indoors and outdoors of old age homes in Antwerp. The case reported here specifically relates to high versus normal/low pollution event periods. PM mass concentrations for PM1 and PM2.5 fractions were determined gravimetrically after collection via impaction. These same samples were hence analysed by EDXRF spectrometry and IC for their elemental and ionic compositions, respectively. During high pollution event days, PM mass concentrations inside the old age home reached 53 μg m− 3 and 32 μg m− 3 whilst outside concentrations were 101 μg m− 3 and 46 μg m− 3 for PM2.5 and PM1, respectively. The sum of nss-sulphate, nitrate and ammonium, dominate the composition of PM, and contribute the most towards an increase in the PM during the episode days constituting 64% of ambient PM2.5 (52 μg m− 3) compared to 39% on non-episode days (10 μg m− 3). Other PM components, such as mineral dust, sea salt or heavy metals were found to be considerably higher during PM episodes but relatively less important. Amongst heavy metals Zn and Pb were found at the highest concentrations in both PM2.5 and PM1. Acidbase ionic balance equations were calculated and point to acidic aerosols during event days and acidic to alkaline aerosols during non-event days. No significant sources of indoor pollutants could be identified inside the old-age home as high correlations were found between outdoor and indoor PM, confirming mainly the outdoor origin of indoor air.

Abstract: The mitigation of pollution released to the environment originating fromthe industrial sector has been the aimof all policy-makers and its importance is evident if the adverse health effects on the world population are considered. Although this concern is controversial, petroleum refinery has been linked to some adverse health effects for people living nearby. Apart from home, school is the most important indoor environment for children and there is increasing concern about the school environment and its impact on health, also in developing countries where the prevalence of pollution is higher. As most of the children spend more than 40% of their time in schools, it is critical to evaluate the pollution level in such environment. In the metropolitan region of Curitiba, South Brazil, five schools nearby industries and highways with high density traffic, were selected to characterize the aerosol and gaseous compounds indoor and outdoor of the classrooms, during 20092011. Size segregated aerosol samples were collected for analyses of bulk and single particle elemental profiles. They were analyzed by electron probe X-ray micro-analysis (EPXMA), and by energy-dispersive X-ray fluorescence (EDXRF), to investigate the elemental composition of individual particles and bulk samples. The concentrations of benzene, toluene, ethylbenzene, and xylene (BTEX); NO2; SO2; acetic acid; and formic acid were assessed indoor and outdoor using passive diffusion tubes. BTEX were analyzed by GCMS and other collected gasses by ion chromatography. Individual exposition of BTEX was assessed by personal passive diffusion tubes. Results are interpreted separately and as a whole with the specific aim of identifying compounds that could affect the health of the scholars. In view of the chemical composition and size distribution of the aerosol particles, local deposition efficiencies in the children's respiratory systems were calculated, revealing the deposition of particles at extrathoracic, tracheobronchial and pulmonary levels.

Abstract: The presence of persistent organic pollutants in Tanzanian environment is not well monitored despite the existing pollution potential from a number of sources. In this study, we investigated for the first time, the concentration profiles of different organohalogen compounds such as organochlorine pesticide residues (OCPs), polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) in environmental samples (water and sediments) from the Pangani river basin (PRB). The PRB is one of the largest drainage basins in Tanzania, with its watershed exposed to multiple input sources of trace organic contaminants. Surface water and sediments were sampled from 12 representative stations of diverse characteristics and land-use practices, in three distinct seasons, and extracted by liquidliquid and Soxhlet extraction methods, respectively. Water samples were analyzed by GC-ECD for OCPs only, while sediment samples were analyzed for OCPs, PCBs and PBDEs by GC/MS. Seven compounds, dominated by HCH isomers (5104460 pg/L) and DDT analogs (1601460 pg/L),were detected in the water samples. These concentrations are far below the WHO guidelines for drinking water quality. A total of 42 compounds (8 OCPs, 28 PCB congeners and 6 PBDE congeners) were detected in the sediment samples. Their respective total concentration ranges were 24510,230; 35711,000 and 382175 pg/g dry weight. The spatial distribution patterns and Hierarchical Cluster Analysis reflected the impact of historical agricultural usage in sugarcane plantations (OCPs), and urbanization (PCBs and PBDEs). Risk assessment using sediment quality guidelines indicated no ecotoxicological risks. The results we have found provide preliminary data on levels of the organic contaminants in Pangani river basin as a new insight on the environmental quality of the area.

Abstract: A variety of samples, collected from different historical buildings and monuments throughout Belgium, were thoroughly studied, using several trace- and micro-analysis techniques. Thin sections of stones and mortar joints were characterized by means of electron probe X-ray microanalysis (EPXMA). The morphological appearance of the surface weathering crust and the possible presence of non-innate particles in the crust were elucidated using petrographical and electron microscopy. Quantitative characterization of the total chemical composition of the crust surface layer and underlying layer was performed by energy-dispersive X-ray fluorescence, and by ion chromatography and atomic absorption spectrometry for the leachable components. Special attention was also paid to the chemical composition of rain and air at the particular sampling sites. The element distribution in the transition zone between the weathering crust and the original stone material was found to vary greatly amongst the different samples analyzed. Detailed EPXMA measurements on pieces of the weathering crust showed remarkable differences in morphology and composition between the surface and the underlying layer, and provided information about the presence of fly-ash and soil dust particles in the crust. Except for crusts from the city of Brussels, which were all very high in sulphate, the samples appeared to contain very variable sulphate contents; very local micro-climate and environmental conditions at a particular site are more important in determining the weathering condition of the building stones than the local air pollution situation. Bulk analytical characterization further showed, in all the crust samples studied, a very small contribution of nitrogen- and chlorine-containing weathering products, in contrast to sulphur-containing weathering salts.