An improved Beenakker-type cavity for microwave induced plasma spectrometry
No abstract available.
Spectrochimica Acta Part B: Atomic Spectroscopy↗
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Iron- and 4-hydroxy-2-alkylquinoline-containing periplasmic inclusion bodies of Pseudomonas aeruginosa: A chemical analysis
Dark aggregated particles were seen on pellets of iron-rich, mid-logarithmic phase Pseudomonas aeruginosa. Transmission electron microscopy of these cells showed inclusion bodies in periplasmic vacuoles. Aggregated particles isolated from the spent medium of these cells contained iron as indicated by atomic absorption spectroscopy and by electron paramagnetic resonance spectroscopy that revealed Fe3+. Scanning electron microscopy/energy dispersive X-ray analysis of whole cells revealed the presence of iron-containing particles beneath the surface of the cell, indicating that the isolated aggregates were the intracellular inclusion bodies. Collectively, mass spectroscopy and nuclear magnetic resonance spectroscopy of the isolated inclusion bodies revealed the presence of 3,4-dihydroxy-2-heptylquinoline which is the Pseudomonas quinolone signaling compound (PQS) and an iron chelator; 4-hydroxy-2-heptylquinoline (pseudan VII), which is an iron chelator, antibacterial compound and precursor of PQS; 4-hydroxy-2-nonylquinoline (pseudan IX) which is an iron chelator and antibacterial compound; 4-hydroxy-2-methylquinoline (pseudan I), and 4-hydroxy-2-nonylquinoline N-oxide. ?? 2006 Elsevier Inc. All rights reserved.
Bioorganic Chemistry↗
Stability of mercury concentration measurements in archived soil and peat samples
Archived soil samples can provide important information on the history of environmental contamination and by comparison with recently collected samples, temporal trends can be inferred. Little previous work has addressed whether mercury (Hg) concentrations in soil samples are stable with long-term storage under standard laboratory conditions. In this study, we have re-analyzed using cold vapor atomic adsorption spectroscopy a set of archived soil samples that ranged from relatively pristine mountainous sites to a polluted site near a non-ferrous metal smelter with a wide range of Hg concentrations (6 - 6485 µg kg-1). Samples included organic and mineral soils and peats with a carbon content that ranged from 0.2 to 47.7%. Soil samples were stored in polyethylene bags or bottles and held in laboratory rooms where temperature was not kept to a constant value. Mercury concentrations in four subsets of samples were originally measured in 2000, 2005, 2006 and 2007, and re-analyzed in 2017, i.e. after 17, 12, 11 and 10 years of storage. Statistical analyses of either separated or lumped data yielded no significant differences between the original and current Hg concentrations. Based on these analyses, we show that archived soil and peat samples can be used to evaluate historical soil mercury contamination.
Chemosphere↗
Biogenic silica in Lake Baikal sediments: results from 1990-1992 American cores
The Lake Baikal Paleoclimate Project is a joint Russian-American program established to study the paleoclimate of Central Asia. During three summer field seasons, duplicate Russian and American cores were taken at a number of sites in different sedimentary environments in the lake. Eight cores returned to the U.S. were quantitatively analyzed for biogenic silica using a single-step 5-hour alkaline leach, followed by dissolved silicon analysis by inductively-coupled-plasma atomic-emission spectroscopy. Sediments of Holocene age in these cores have biogenic silica maxima that range from about 15 to 80 percent. An underlying zone in each core with low biogenic-silica concentrations (0 to 5 percent) dates from the last glacial maximum. The transition from the last glaciation to the present interglaciation, recorded by biogenic silica, began about 13,000 years ago. Biogenic silica profiles from these cores appear to be a good measure of past diatom productivity and a useful basis for paleoclimatic interpretations.
Lake Baikal↗
Copper localization, elemental content, and thallus colour in the copper hyperaccumulator lichen Lecanora sierrae from California
An unusual dark blue-green lichen, Lecanora sierrae , was discovered over 30 years ago by Czehura near copper mines in the Lights Creek District, Plumas County, Northern California. Using atomic absorption spectroscopy, Czehura found that dark green lichen samples from Warren Canyon contained 4% Cu in ash and suggested that its colour was due to copper accumulation in the cortex. The present study addressed the hypothesis that the green colour in similar material we sampled from Warren Canyon in 2008, is caused by copper localization in the thallus. Optical microscopy and electron microprobe analysis of specimens of L. sierrae confirmed that copper localization took place in the cortex. Elemental analyses of L. sierrae and three other species from the same localities showed high enrichments of copper and selenium, suggesting that copper selenates or selenites might occur in these lichens and be responsible for the unusual colour.
Lichenologist↗
Freshwater mussel shells as environmental chronicles: Geochemical and taphonomic signatures of mercury-related extirpations in the North Fork Holston River, Virginia
This study utilized freshwater mussel shells to assess mercury (Hg) contamination in the North Fork Holston River that extirpated (caused local extinctions of) a diverse mussel fauna. Shells (n = 366) were collected from five sites situated upstream (two sites), just below (one site), and downstream (two sites) of the town of Saltville, Virginia, where Hg was used to produce chlorine and caustic soda from 1950 to 1972. Shell samples were used to test the (1) utility of geochemical signatures of shells for assessing the spatial variation in Hg levels in the river relative to the contamination source and (2) value of taphonomy (postmortem shell alteration) for distinguishing sites that differ in extirpation histories. Geochemical signatures of 40 shells, analyzed using atomic absorption spectroscopy, indicated a strong longitudinal pattern. All shells from the two upstream sites had low Hg concentrations (<5-31 ??g/kg), shells directly below Saltville had variable, but dramatically higher concentrations (23-4637 ??g/kg), and shells from the two downstream sites displayed intermediate Hg levels (<5-115 ??g/kg) that declined with distance from Saltville. Two pre-industrial shells, collected at Saltville in 1917, yielded very low Hg estimates (5-6 ??g/kg). Hg signatures were consistent among mussel species, suggesting that Hg concentrations were invariant to species type; most likely, highly variable Hg levels, both across sites and through time, overwhelmed any interspecific differences in Hg acquisition. Also, a notable postmortem incorporation of Hg in mussel shells seemed unlikely, as the Hg content was not correlated with shell taphonomy (r = 0.18; p = 0.28). The taphonomic analysis (n = 366) showed that the degree of shell alteration reliably distinguished sites with different extirpation histories. At Saltville, where live mussels have been absent for at least 30 years, shells were most heavily altered and fragmented. Conversely, fresh-looking shells abounded upstream, where reproducing mussel populations are still present. In summary, relic shells offered valuable spatiotemporal data on Hg concentrations in a polluted ecosystem, and shell taphonomic signatures discriminated sites with different extirpation histories. The shell-based strategies exemplified here do not require sampling live specimens and may augment more standard strategies applied to environmental monitoring. The approach should prove especially useful in areas with unknown extirpation and pollution histories. ?? 2005 American Chemical Society.
Environmental Science & Technology↗
Silica-coated titania and zirconia colloids for subsurface transport field experiments
Silica-coated titania (TiO 2 ) and zirconia (ZrO 2 ) colloids were synthesized in two sizes to provide easily traced mineral colloids for subsurface transport experiments. Electrophoretic mobility measurements showed that coating with silica imparted surface properties similar to pure silica to the titania and zirconia colloids. Measurements of steady electrophoretic mobility and size (by dynamic light scattering) over a 90-day period showed that the silica-coated colloids were stable to aggregation and loss of coating. A natural gradient field experiment conducted in an iron oxide-coated sand and gravel aquifer also showed that the surface properties of the silica-coated colloids were similar. Colloid transport was traced at μg L - 1 concentrations by inductively coupled plasma-atomic emission spectroscopy measurement of Ti and Zr in acidified samples.
Environmental Science & Technology↗
Concentrations of arsenic, cadmium, copper, lead, selenium, and zinc in fish from the Mississippi River Basin, 1995
Fish were collected in late 1995 from 34 National Contaminant Biomonitoring Program (NCBP) stations and 12 National Water Quality Assessment Program (NAWQA) stations in the Mississippi River basin (MRB), and in late 1996 from a reference site in West Virginia. The NCBP sites represented key points (dams, tributaries, etc.) in the largest rivers of the MRB. The NAWQA sites were typically on smaller rivers and were selected to represent dominant land uses in their watersheds. The West Virginia site, which is in an Eastern U.S. watershed adjacent to the MRB, was selected to document elemental concentrations in fish used for other aspects of a larger study and to provide additional contemporaneous data on background elemental concentrations. At each site four samples, each comprising (nominally) 10 adult common carp ( Cyprinus carpio , `carp') or black bass ( Micropterus spp., `bass') of the same sex, were collected. The whole fish were composited by station, species, and gender for analysis of arsenic (As), lead (Pb), and selenium (Se) by atomic absorption spectroscopy and for cadmium (Cd), copper (Cu), and zinc (Zn) by inductively-coupled plasma emission spectroscopy. Concentrations of most of the elements examined were lower in both carpand bass from the reference site, a small impoundment located in a rural area, than from the NCBP and NAWQA sites on rivers and larger impoundments. In contrast, there were few overall differences between NCBP sites NAWQA sites. The 1995 results generally confirmed the continued weathering and re-distribution of these elemental contaminants in the MRB; concentrations declined or were unchanged from 1984–1986 to 1995 at most NCBP sites, thus continuing two-decade trends. Exceptions were Se at Station 77 (Arkansas R. at John Martin Reservoir, CO), where concentrations have been elevated historically and increased slightly (to 3.8–4.7 μg g -1 in bass and carp); and Pb, Cd, and Zn at Station 67 (Allegheny R. at Natrona, PA), where levels of these metals were high in the past and increased from 1986 to 1995.
Environmental Monitoring and Assessment↗
Mineralogy and arsenic mobility in arsenic-rich Brazilian soils and sediments
Background. Soils and sediments in certain mining regions of Brazil contain an unusually large amount of arsenic (As), which raises concerns that mining could promote increased As mobility, and thereby increase the risks of contaminating water supplies. Objectives. The purpose of t his study was to identify the most important factors governing As mobility in sediments and soils near three gold-mining sites in the State of Minas Gerais, Brazil. Methods. Surface and sub-surface soil samples were collected at those sites and characterized by chemical and mineralogical analyses. Oxalate (Feo) and citrate-bicarbonate-dithionite (Fed) iron contents were determined by atomic absorption spectroscopy (AAS). Arsenic mobilization was measured after incubating the samples in a 2.5 mM CaCl2 solution under anaerobic conditions for 1, 28, 56, 84, or 112 days. The solution concentrations of As, Fe, and Mn were then measured by inductively coupled plasma-mass spectrometry (ICP-MS) and AAS, respectively. Results and Discussion. Results indicated that As mobilization is largely independent of both the total As and the Feo/Fed ratio of the solid phase. Soluble As is roughly controlled by the Fe (hydr)oxide content of the soil, but a closer examination of the data revealed the importance of other highly weathered clay minerals and organic matter. Large amounts of organic matter and a low iron oxide content should favor As leaching from soils and sediments. Under reducing conditions, As is mobilized by the reductive dissolution of Fe and/or Mn oxides. However, released As may be readsorbed depending on the sorptive properties of the soil. Gibbsite is particularly effective in adsorbing or readsorbing As, as is the remaining unreduced fraction of the iron (hydr)oxides. Conclusion and Outlook. In general, low soluble As is rel ated to the presence of gibbsite, a large amount of iron oxides, and a lack of organic matter in the solid phase. This has environmental significance because gibbsite is thermodynamically more stable than Fe oxides under anaerobic conditions, such as those found in waterlogged soils and lake sediments. ?? 2006 ecomed publishers (Verlagsgruppe Hu??thig Jehle Rehm GmbH), D-86899 Landsberg and Tokyo.
Journal of Soils and Sediments↗
Guidelines for sample collecting and analytical methods used in the U.S. Geological Survey for determining chemical composition of coal
This report is intended to meet the many requests for information on current U.S. Geological Survey procedures in handling coal samples. In general, the exact type and number of samples of coal and associated rock to be collected are left to the best judgment of the geologist. Samples should be of unweathered coal or rock and representative of the bed or beds sampled; it is recommended that two channel samples, separated by 10 to 100 yards (10 to 100 metres) and weighing 4 to 5 pounds ( 1.8 to 2.3 kilograms) each, be collected of each 5 feet ( 1.5 metres) of vertical section. Care must be taken to avoid any sample contamination, and to record the exact locality, thickness, and stratigraphic information for each sample. Analytical methods are described for the determination of major, minor, and trace elements in coal. Hg, As, Sb, F, Se, U, and Th are determined in the raw coal, and the following 34 elements are determined after ashing the coal: Si, Al, Ca, Mg, Na, K, Fe (total), Cl, Ti, Mn, P, S (total), Cd, Li, Cu, Zn, Pb, B, Ba, Be, Co, Cr, Ga, La, Mo, Nb, Ni, Sc, Sr, Ti, V, Y, Yb, and Zr. The methods used to determine these elements include atomic absorption spectroscopy, X-ray fluorescence spectroscopy, optical emission spectroscopy, spectrophotometry, selective-ion electrode, and neutron activation analysis. A split of representative coal samples is submitted to the U.S. Bureau of Mines for proximate, ultimate, forms of sulfur, and Btu determinations.
Circular↗
Analytical results for Bullion Mine and Crystal Mine waste samples and bed sediments from a small tributary to Jack Creek and from Uncle Sam Gulch, Boulder River watershed, Montana
Metal-mining related wastes in the Boulder River basin study area in northern Jefferson County, Montana affect water quality as a result of acid-generation and toxic-metal solubilization. Mine waste and tailings in the unnamed tributary to Jack Creek draining the Bullion mine area and in Uncle Sam Gulch below the Crystal mine are contributors to water quality degradation of Basin Creek and Cataract Creek, Montana. Basin Creek and Cataract Creek are two of three tributaries to the Boulder River in the study area. The bed sediment geochemistry in these two creeks has also been affected by the acidic drainage from these two mines. Geochemical analysis of 42 tailings cores and eleven bed-sediment samples was undertaken to determine the concentrations of Ag, As, Cd, Cu, Pb, and Zn present in these materials. These elements are environmentally significant, in that they can be toxic to fish and/or the invertebrate organisms in the aquatic food chain. Suites of one-inch cores of mine waste and tailings material were taken from two breached tailings impoundments near the site of the Bullion mine and from Uncle Sam Gulch below the Crystal mine. Forty-two core samples were taken and divided into 211 subsamples. The samples were analyzed by ICP-AES (inductively coupled plasma-atomic emission spectroscopy) using a mixed-acid (HC1-HNO 3 -HC1O 4 -HF) digestion. Results of the core analyses show that some samples contain moderate to very high concentrations of arsenic (as much as 13,000 ppm), silver (as much as 130 ppm), cadmium (as much as 260 ppm), copper (as much as 9,000 ppm), lead (as much as 11,000 ppm), and zinc (as much as 18,000 ppm). Eleven bed-sediment samples were also subjected to the mixed-acid total digestion, and a warm (50°C) 2M HC1-1% H 2 O 2 leach and analyzed by ICP-AES. Results indicate that bed sediments of the Jack Creek tributary are impacted by past mining at the Bullion and Crystal mines. The contaminating metals are mostly contained in the 2M HC1-1% H 2 O 2 leachable phase, which are the hydrous amorphous iron- and manganese-hydroxide coatings on detrital sediment particles.
Montana↗
Determination of methyl mercury by aqueous phase ethylation, followed by gas chromatographic separation with cold vapor atomic fluorescence detection
A recent national sampling of streams in the United States revealed low methyl mercury concentrations in surface waters. The resulting median and mean concentrations, calculated from 104 samples, were 0.06 nanograms per liter (ng/L) and 0.15 ng/L, respectively. This level of methyl mercury in surface water in the United States has created a need for analytical techniques capable of detecting sub-nanogram per liter concentrations. In an attempt to create a U.S. Geological Survey approved method, the Wisconsin District Mercury Laboratory has adapted a distillation/ethylation/ gas-phase separation method with cold vapor atomic fluorescence spectroscopy detection for the determination of methyl mercury in filtered and unfiltered waters. This method is described in this report. Based on multiple analyses of surface water and ground-water samples, a method detection limit of 0.04 ng/L was established. Precision and accuracy were evaluated for the method using both spiked and unspiked ground-water and surface-water samples. The percent relative standard deviations ranged from 10.2 to 15.6 for all analyses at all concentrations. Average recoveries obtained for the spiked matrices ranged from 88.8 to 117 percent. The precision and accuracy ranges are within the acceptable method-performance limits. Considering the demonstrated detection limit, precision, and accuracy, the method is an effective means to quantify methyl mercury in waters at or below environmentally relevant concentrations
Open-File Report↗
Major- and Trace-Element Concentrations in Rock Samples Collected in 2005 from the Taylor Mountains 1:250,000-scale Quadrangle, Alaska
The data consist of major- and minor-element concentrations for rock samples collected during 2005 by the U.S. Geological Survey. Samples were analyzed by fire assay (Au, Pd, Pt), cold vapor atomic absorption spectroscopy (Hg), and the inductively coupled plasma mass spectrometry (ICPMS) 10 and 42 element methods. For details of sample preparation and analytical techniques see USGS Open File Report 02-0223 (Analytical methods for chemical analysis of geologic and other materials, U.S. Geological Survey), available at .
Open-File Report↗
Determination of total mercury in whole-body fish and fish muscle plugs collected from the South Fork of the Humboldt River, Nevada, September 2005
This report presents the results of a study by the U.S. Geological Survey, done in cooperation with the U.S. Bureau of Reclamation, to determine mercury concentrations in whole-body fish and fish muscle plugs from the South Fork of the Humboldt River near Elko in the Te-Moak Indian Reservation. A single muscle plug was collected from beneath the dorsal fin area in each of the three whole-body fish samples. After homogenization and lyophilization of the muscle plugs and whole-body fish samples, mercury concentrations were determined with a direct mercury analyzer utilizing the process of thermal combustion-gold amalgamation atomic absorption spectroscopy. Mercury concentrations in whole-body fish ranged from 0.048 to 0.061 microgram per gram wet weight, and 0.061 to 0.082 microgram per gram wet weight in muscle plugs. All sample mercury concentrations were well below the U.S. Environmental Protection Agency's fish consumption advisory of 0.30 microgram per gram wet weight.
Open-File Report↗
Determination of total mercury in fillets of sport fishes collected from Folsom and New Melones Reservoirs, California, 2004
This report presents the results of a study by the U.S. Geological Survey, done in cooperation with the U.S. Bureau of Reclamation, to determine mercury concentrations in selected sport fishes from Folsom and New Melones Reservoirs in California. Fillets were collected from each fish sample, and after homogenization and lyophilization of fish fillets, mercury concentrations were determined with a direct mercury analyzer utilizing the process of thermal combustion-gold amalgamation atomic absorption spectroscopy. Mercury concentrations in fish fillets from Folsom Reservoir ranged from 0.09 to 1.16 micrograms per gram wet weight, and from New Melones Reservoir ranged from 0.03 to 0.94 microgram per gram wet weight. Most of the fish fillets from Folsom Reservoir (87 percent) and 27 percent of the fillets from New Melones Reservoir exceeded the U.S. Environmental Protection Agency's fish consumption advisory of 0.30 microgram per gram wet weight.
Open-File Report↗
Determination of total mercury in fillets of sport fishes collected from Folsom Reservoir, California, 2006
This report presents the results of a study by the U.S. Geological Survey, done in cooperation with the U.S. Bureau of Reclamation, to determine mercury concentrations in selected sport fishes from Folsom Reservoir in California. Fillets were collected from each fish sample, and after homogenization and lyophilization of fish fillets, mercury concentrations were determined with a direct mercury analyzer utilizing the process of thermal combustion-gold amalgamation atomic absorption spectroscopy. Mercury concentrations in fillets ranged from 0.031 to 0.20 micrograms per gram wet weight in rainbow trout (Oncorhynchus mykiss) samples and 0.071 to 0.16 micrograms per gram wet weight in bluegill (Lepomis macrochirus) samples. Mercury concentration was 0.98 microgram per gram wet weight in a single spotted bass (Micropterus punctulatus) sample, which was the only one in the sample set which exceeded the U.S. Environmental Protection Agency's fish consumption advisory of 0.30 microgram per gram wet weight.
Open-File Report↗
Chemical data for precipitate samples
During studies of sulfide oxidation in coastal areas of Prince William Sound in 2005, precipitate samples were collected from onshore and intertidal locations near the Ellamar, Threeman, and Beatson mine sites (chapter A, fig. 1; table 7). The precipitates include jarosite and amorphous Fe oxyhydroxide from Ellamar, amorphous Fe oxyhydroxide from Threeman, and amorphous Fe oxyhydroxide, ferrihydrite, and schwertmannite from Beatson. Precipitates occurring in the form of loose, flocculant coatings were harvested using a syringe and concentrated in the field by repetitive decanting. Thicker accumulations were either scraped gently from rocks using a stainless steel spatula or were scooped directly into receptacles (polyethylene jars or plastic heavy-duty zippered bags). Most precipitate samples contain small amounts of sedimentary detritus. With three jarosite-bearing samples from Ellamar, an attempt was made to separate the precipitate from the heavy-mineral fraction of the sediment. In this procedure, the sample was stirred in a graduated cylinder containing deionized water. The jarosite-rich suspension was decanted onto analytical filter paper and air dried before analysis. Eleven precipitate samples from the three mine sites were analyzed in laboratories of the U.S. Geological Survey (USGS) in Denver, Colorado (table 8). Major and trace elements were determined by inductively coupled plasma-mass spectrometry following multiacid (HCl-HNO3-HClO4-HF) digestion (Briggs and Meier, 2002), except for mercury, which was analyzed by cold-vapor atomic absorption spectroscopy (Brown and others, 2002a). X-ray diffraction (XRD) analyses were performed on powdered samples (<200 mesh) by S. Sutley of the USGS. Additional details regarding sample preparation and detection limits are found in Taggert (2002). Discussions of the precipitate chemistry and associated microbial communities are presented in Koski and others (2008) and Foster and others (2008), respectively.
Alaska↗
Concentrations of mercury and other metals in black bass (Micropterus spp.) from Whiskeytown Lake, Shasta County, California, 2005
This report presents the results of a reconnaissance study conducted by the U.S. Geological Survey (USGS) to determine mercury (Hg) and other selected metal concentrations in Black bass ( Micropterus spp. ) from Whiskeytown Lake, Shasta County, California. Total mercury concentrations were determined by cold-vapor atomic absorption spectroscopy (CVAAS) in fillets and whole bodies of each sampled fish. Selected metals scans were performed on whole bodies (less the fillets) by inductively coupled plasma–mass spectroscopy (ICP-MS) and inductively coupled plasma–optical emission spectroscopy (ICP-OES). Mercury concentrations in fillet samples ranged from 0.06 to 0.52 micrograms per gram (μg/g) wet weight (ww). Total mercury (HgT) in the same fish whole-body samples ranged from 0.04 to 0.37 (μg/g, ww). Mercury concentrations in 17 percent of "legal catch size" (≥305 millimeters in length) were above the U.S. Environmental Protection Agency water-quality criterion for the protection of human health of 0.30 μg/g (ww). These data will serve as a baseline for future monitoring efforts within Whiskeytown Lake.
California↗