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The determination of vanadium in brines by atomic absorption spectroscopy

A standard addition method is described for the determination of vanadium in brines by atomic absorption spectroscopy with a nitrous oxide-acetylene flame. Sample pH is adjusted to 1.0 with concentrated hydrochloric acid and the vanadium is directly extracted with 5% cupferron in methyl isobutyl ketone (MIBK). The ketone layer is then aspirated into the flame and the recorded absorption values are plotted as a function of the concentration of the added metal. As little as 2.5 μg l −1 of vanadium can be detected under the conditions of the procedure. Tungsten and tin interfere when present in excess of 5 and 10 μg ml −1 , respectively. The concentrations of the two interfering ions normally found in brines are well below interference levels.

Analytica Chimica Acta

An improved method for the determination of trace levels of arsenic and antimony in geological materials by automated hydride generation–Atomic absorption spectroscopy

An improved, automated method for the determination of arsenic and antimony in geological materials is described. After digestion of the material in sulfuric, nitric, hydrofluoric and perchloric acids, a hydrochloric acid solution of the sample is automatically mixed with reducing agents, acidified with additional hydrochloric acid, and treated with a sodium tetrahydroborate solution to form arsine and stibine. The hydrides are decomposed in a heated quartz tube in the optical path of an atomic absorption spectrometer. The absorbance peak height for arsenic or antimony is measured. Interferences that exist are minimized to the point where most geological materials including coals, soils, coal ashes, rocks and sediments can be analyzed directly without use of standard additions. The relative standard deviation of the digestion and the instrumental procedure is less than 2% at the 50 μg l -1 As or Sb level. The reagent-blank detection limit is 0.2 μg l -1 As or Sb.

Analytica Chimica Acta

Determination of gold, indium, tellurium and thallium in the same sample digest of geological materials by atomic-absorption spectroscopy and two-step solvent extraction

A rock, soil, or stream-sediment sample is decomposed with hydrofluoric acid, aqua regia , and hydrobromic acid-bromine solution. Gold, thallium, indium and tellurium are separated and concentrated from the sample digest by a two-step MIBK extraction at two concentrations of hydrobromic add. Gold and thallium are first extracted from 0.1 M hydrobromic acid medium, then indium and tellurium are extracted from 3 M hydrobromic acid in the presence of ascorbic acid to eliminate iron interference. The elements are then determined by flame atomic-absorption spectrophotometry. The two-step solvent extraction can also be used in conjunction with electrothermal atomic-absorption methods to lower the detection limits for all four metals in geological materials.

Talanta

A rapid method for determining tin and molybdenum in geological samples by flame atomic-absorption spectroscopy

The proposed method uses a lithium metaborate fusion, dissolution of the fusion bead in 15% vv hydrochloric acid, extraction into a 4% solution of trioctylphosphine oxide in methyl isobutyl ketone, and aspiration into a nitrous oxide-acetylene flame. The limits of detection for tin and molybdenum are 1.0 and 0.5 ppm, respectively. Approximately 50 samples can be analysed per day.

Talanta

Multielement extraction system for determining 19 trace elements in gold exploration samples

A multielement extraction system is being used successfully to provide essentially interference-free geochemical analyses to aid in gold exploration. The Methyl isobutyl ketone-Amine synerGistic Iodide Complex (MAGIC) extraction system separates Ag, As, Au, Bi, Cd, Cu, Ga, Hg, In, Mo, Pb, Pd, Pt, Sb, Se, Sn, Te, Tl, and Zn from interfering geological matrices. Quantitative extraction of these elements is accomplished over a broad range of acid normality making it possible to economically determine all 19 elements from a single digestion or leach solution. The resulting organic extracts are amenable to analysis by inductively coupled plasma atomic emission spectroscopy (ICP-AES) and flame atomic absorption spectroscopy (FAAS). For many years the principal shortcoming of ICP-AES was the complex spectral and stray-light interferences that were caused by the extreme variability of components such as Fe, Na, and Ca in common geological matrices. The MAGIC extraction allows determination of the extracted elements with enhanced sensitivity, from a virtually uniform matrix, by ICP-AES and FAAS. Because of its simultaneous multichannel capabilities, ICP-AES is the ideal instrumental technique for determining these 19 extracted elements. Ultratrace (sub-part-per-billion) determinations of Au and many of the other extracted elements can be made by graphite furnace atomic absorption spectroscopy (GFAAS), following back stripping of the extracts. The combination of the extraction followed by stripping of the organic phase eliminates 99.999% of potential interferences for Au. Gold determination by GFAAS from these extracts under the specified conditions yields a fourfold improvement in sensitivity over conventional GFAAS methods. This sensitivity enhancement and the interference-free matrix allow highly reliable determinations well into the parts-per-trillion range.

Conference Paper

Thallium contents of 16 USGS standard rocks

Thallium was determined in 16 USGS standard rocks by atomic absorption spectroscopy in which a heated graphite atomizer was used after extraction as thallium iodide into amyl acetate. Four subsamples from four bottles of each standard sample, except G-1 and W-1, were analyzed in random order, and the average thallium contents in parts per million (as Tl) were AGV-1, 0.41; GSP-1, 1.63; G-2, 1.08; BCR-1, 0.35; SDC-1, 0.80; MAG-1, 0.79; BHVO-1, 0.049; SCO-1, 0.79; SGR-1, 0.34; QLO-1, 0.23; RGM-1, 1.07 ; STM-1, 0.30; DTS-1, <0.005; and PCC-1, <0.005. The analysis of variance showed that all samples may be considered homogeneous at F 0.975 and only GSP-1 may be considered heterogeneous at F 0.95 . The Tl contents of G-1 and W-1 are 1.0 and 0.12 ppm, respectively.

Journal of Research of the U.S. Geological Survey

The determination of Metals in sediment pore waters and in 1N HCl-extracted sediments by ICP-MS

Concentrations of metals in sediment interstitial water (pore water) and those extractable from sediment with weak acids can provide important information about the bioavailability and toxicological effects of such contaminants. The highly variable nature of metal concentrations in these matrices requires instrumentation with the detection limit capability of graphite furnace atomic absorption and the wide dynamic linear range capability of ICP-OES. These criteria are satisfied with ICP-MS instrumentation. We investigated the performance of ICP-MS in the determination of certain metals from these matrices. The results for three metals were compared to those determined by graphite furnace atomic absorption spectroscopy. It was concluded that ICP-MS was an excellent instrumental approach for the determination of metals in these matrices.

Atomic Spectroscopy

Part A: Geochemistry of Soil Samples from 50 Solution-Collapse Features on the Coconino Plateau, Northern Arizona

Soil sampling surveys were conducted during 1984-1986 across 50 solution-collapse features exposed on the Coconino Plateau of northern Arizona in order to determine whether soil geochemistry can be used to distinguish mineralized breccia pipes from unmineralized collapse features. The 50 sampled features represent the variety of collapse features that crop out on plateau surfaces in northwestern Arizonaoodeeplyorooted solution-collapse breccia pipes, near-surface gypsum collapses, and sinkholes. Of the 50 features that were sampled in this study, 3 are confirmed breccia pipes that contain significant uranium and base-metal minerals, I is believed to be a sinkhole with no economic potential, and 4 are stratabound copper deposits whose possible relationship to breccia pipes is yet to be determined. The remaining collapse features are suspected to overlie breccia pipes, although some of these may represent near surface gypsum collapse features. However, no exploratory drilling results or breccia exposures exist to indicate their underlying structure. The low cost and ease of soil sampling suggested that this technique be evaluated for breccia pipe exploration. This report provides the locations and geochemical results for the soil sampling surveys and brief descriptions of the 50 collapse features. The analytical results of almost 2,000 soil samples are provided in tabular hardcopy and dBase III Plus diskcopy format. The analytical data is provided in digital format to allow the reader to choose their own methods for evaluating the effectiveness of soil sampling over known and suspected breccia pipes. A pilot survey conducted over 17 collapse features in 1984 suggested that soil sampling might be useful in distinguishing mineralized breccia pipes from other circular features. Followup detailed surveys in 1985 and 1986 used a radial sampling pattern at each of 50 sites; at least one third of the samples were collected from areas outside of the collapse feature to provide background data. Samples were consistently collected from 3-4 inches depth after the pilot survey showed that metal concentrations were similar in samples from 3-4 inches and 7-8 inches depth. The geochemical analyses of the <80 mesh fractions of the soil samples were performed by the U.S. Geological Survey Analytical Laboratories and Geochemical Services, Inc. The analytical methods applied to these samples by the U.S. Geological Survey laboratories included inductively coupled plasma-atomic emission spectroscopy, X-ray fluorescence spectrometry, neutron activation, atomic absorption, delayed neutron activation, and classical wet chemistry for carbon, fluorine, and sulfur. Geochemical Services, Inc. analyzed the soil samples by inductively coupled plasma emission spectroscopy.

Open-File Report

Geochemistry of Soil Samples from 50 Solution-Collapse Features on the Coconino Plateau, Northern Arizona

Soil sampling surveys were conducted during 1984-1986 across 50 solution-collapse features exposed on the Coconino Plateau of northern Arizona in order to determine whether soil geochemistry can be used to distinguish mineralized breccia pipes from unmineralized collapse features. The 50 sampled features represent the variety of collapse features that crop out on plateau surfaces in northwestern Arizonaoodeeplyorooted solution-collapse breccia pipes, near-surface gypsum collapses, and sinkholes. Of the 50 features that were sampled in this study, 3 are confirmed breccia pipes that contain significant uranium and base-metal minerals, I is believed to be a sinkhole with no economic potential, and 4 are stratabound copper deposits whose possible relationship to breccia pipes is yet to be determined. The remaining collapse features are suspected to overlie breccia pipes, although some of these may represent near surface gypsum collapse features. However, no exploratory drilling results or breccia exposures exist to indicate their underlying structure. The low cost and ease of soil sampling suggested that this technique be evaluated for breccia pipe exploration. This report provides the locations and geochemical results for the soil sampling surveys and brief descriptions of the 50 collapse features. The analytical results of almost 2,000 soil samples are provided in tabular hardcopy and dBase III Plus diskcopy format. The analytical data is provided in digital format to allow the reader to choose their own methods for evaluating the effectiveness of soil sampling over known and suspected breccia pipes. A pilot survey conducted over 17 collapse features in 1984 suggested that soil sampling might be useful in distinguishing mineralized breccia pipes from other circular features. Followup detailed surveys in 1985 and 1986 used a radial sampling pattern at each of 50 sites; at least one third of the samples were collected from areas outside of the collapse feature to provide background data. Samples were consistently collected from 3-4 inches depth after the pilot survey showed that metal concentrations were similar in samples from 3-4 inches and 7-8 inches depth. The geochemical analyses of the <80 mesh fractions of the soil samples were performed by the U.S. Geological Survey Analytical Laboratories and Geochemical Services, Inc. The analytical methods applied to these samples by the U.S. Geological Survey laboratories included inductively coupled plasma-atomic emission spectroscopy, X-ray fluorescence spectrometry, neutron activation, atomic absorption, delayed neutron activation, and classical wet chemistry for carbon, fluorine, and sulfur. Geochemical Services, Inc. analyzed the soil samples by inductively coupled plasma emission spectroscopy.

Open-File Report

Part B: Geochemistry of Soil Samples from 50 Solution-Collapse Features on the Coconino Plateau, Northern Arizona

Soil sampling surveys were conducted during 1984-1986 across 50 solution-collapse features exposed on the Coconino Plateau of northern Arizona in order to determine whether soil geochemistry can be used to distinguish mineralized breccia pipes from unmineralized collapse features. The 50 sampled features represent the variety of collapse features that crop out on plateau surfaces in northwestern Arizonaoodeeplyorooted solution-collapse breccia pipes, near-surface gypsum collapses, and sinkholes. Of the 50 features that were sampled in this study, 3 are confirmed breccia pipes that contain significant uranium and base-metal minerals, I is believed to be a sinkhole with no economic potential, and 4 are stratabound copper deposits whose possible relationship to breccia pipes is yet to be determined. The remaining collapse features are suspected to overlie breccia pipes, although some of these may represent near surface gypsum collapse features. However, no exploratory drilling results or breccia exposures exist to indicate their underlying structure. The low cost and ease of soil sampling suggested that this technique be evaluated for breccia pipe exploration. This report provides the locations and geochemical results for the soil sampling surveys and brief descriptions of the 50 collapse features. The analytical results of almost 2,000 soil samples are provided in tabular hardcopy and dBase III Plus diskcopy format. The analytical data is provided in digital format to allow the reader to choose their own methods for evaluating the effectiveness of soil sampling over known and suspected breccia pipes. A pilot survey conducted over 17 collapse features in 1984 suggested that soil sampling might be useful in distinguishing mineralized breccia pipes from other circular features. Followup detailed surveys in 1985 and 1986 used a radial sampling pattern at each of 50 sites; at least one third of the samples were collected from areas outside of the collapse feature to provide background data. Samples were consistently collected from 3-4 inches depth after the pilot survey showed that metal concentrations were similar in samples from 3-4 inches and 7-8 inches depth. The geochemical analyses of the <80 mesh fractions of the soil samples were performed by the U.S. Geological Survey Analytical Laboratories and Geochemical Services, Inc. The analytical methods applied to these samples by the U.S. Geological Survey laboratories included inductively coupled plasma-atomic emission spectroscopy, X-ray fluorescence spectrometry, neutron activation, atomic absorption, delayed neutron activation, and classical wet chemistry for carbon, fluorine, and sulfur. Geochemical Services, Inc. analyzed the soil samples by inductively coupled plasma emission spectroscopy.

Open-File Report

Part C: Geochemistry of Soil Samples from 50 Solution-Collapse Features on the Coconino Plateau, Northern Arizona

Soil sampling surveys were conducted during 1984-1986 across 50 solution-collapse features exposed on the Coconino Plateau of northern Arizona in order to determine whether soil geochemistry can be used to distinguish mineralized breccia pipes from unmineralized collapse features. The 50 sampled features represent the variety of collapse features that crop out on plateau surfaces in northwestern Arizonaoodeeplyorooted solution-collapse breccia pipes, near-surface gypsum collapses, and sinkholes. Of the 50 features that were sampled in this study, 3 are confirmed breccia pipes that contain significant uranium and base-metal minerals, I is believed to be a sinkhole with no economic potential, and 4 are stratabound copper deposits whose possible relationship to breccia pipes is yet to be determined. The remaining collapse features are suspected to overlie breccia pipes, although some of these may represent near surface gypsum collapse features. However, no exploratory drilling results or breccia exposures exist to indicate their underlying structure. The low cost and ease of soil sampling suggested that this technique be evaluated for breccia pipe exploration. This report provides the locations and geochemical results for the soil sampling surveys and brief descriptions of the 50 collapse features. The analytical results of almost 2,000 soil samples are provided in tabular hardcopy and dBase III Plus diskcopy format. The analytical data is provided in digital format to allow the reader to choose their own methods for evaluating the effectiveness of soil sampling over known and suspected breccia pipes. A pilot survey conducted over 17 collapse features in 1984 suggested that soil sampling might be useful in distinguishing mineralized breccia pipes from other circular features. Followup detailed surveys in 1985 and 1986 used a radial sampling pattern at each of 50 sites; at least one third of the samples were collected from areas outside of the collapse feature to provide background data. Samples were consistently collected from 3-4 inches depth after the pilot survey showed that metal concentrations were similar in samples from 3-4 inches and 7-8 inches depth. The geochemical analyses of the <80 mesh fractions of the soil samples were performed by the U.S. Geological Survey Analytical Laboratories and Geochemical Services, Inc. The analytical methods applied to these samples by the U.S. Geological Survey laboratories included inductively coupled plasma-atomic emission spectroscopy, X-ray fluorescence spectrometry, neutron activation, atomic absorption, delayed neutron activation, and classical wet chemistry for carbon, fluorine, and sulfur. Geochemical Services, Inc. analyzed the soil samples by inductively coupled plasma emission spectroscopy.

Open-File Report

Part D: Geochemistry of Soil Samples from 50 Solution-Collapse Features on the Coconino Plateau, Northern Arizona

Soil sampling surveys were conducted during 1984-1986 across 50 solution-collapse features exposed on the Coconino Plateau of northern Arizona in order to determine whether soil geochemistry can be used to distinguish mineralized breccia pipes from unmineralized collapse features. The 50 sampled features represent the variety of collapse features that crop out on plateau surfaces in northwestern Arizonaoodeeplyorooted solution-collapse breccia pipes, near-surface gypsum collapses, and sinkholes. Of the 50 features that were sampled in this study, 3 are confirmed breccia pipes that contain significant uranium and base-metal minerals, I is believed to be a sinkhole with no economic potential, and 4 are stratabound copper deposits whose possible relationship to breccia pipes is yet to be determined. The remaining collapse features are suspected to overlie breccia pipes, although some of these may represent near surface gypsum collapse features. However, no exploratory drilling results or breccia exposures exist to indicate their underlying structure. The low cost and ease of soil sampling suggested that this technique be evaluated for breccia pipe exploration. This report provides the locations and geochemical results for the soil sampling surveys and brief descriptions of the 50 collapse features. The analytical results of almost 2,000 soil samples are provided in tabular hardcopy and dBase III Plus diskcopy format. The analytical data is provided in digital format to allow the reader to choose their own methods for evaluating the effectiveness of soil sampling over known and suspected breccia pipes. A pilot survey conducted over 17 collapse features in 1984 suggested that soil sampling might be useful in distinguishing mineralized breccia pipes from other circular features. Followup detailed surveys in 1985 and 1986 used a radial sampling pattern at each of 50 sites; at least one third of the samples were collected from areas outside of the collapse feature to provide background data. Samples were consistently collected from 3-4 inches depth after the pilot survey showed that metal concentrations were similar in samples from 3-4 inches and 7-8 inches depth. The geochemical analyses of the <80 mesh fractions of the soil samples were performed by the U.S. Geological Survey Analytical Laboratories and Geochemical Services, Inc. The analytical methods applied to these samples by the U.S. Geological Survey laboratories included inductively coupled plasma-atomic emission spectroscopy, X-ray fluorescence spectrometry, neutron activation, atomic absorption, delayed neutron activation, and classical wet chemistry for carbon, fluorine, and sulfur. Geochemical Services, Inc. analyzed the soil samples by inductively coupled plasma emission spectroscopy.

Open-File Report

Concentrations of metals in blood and feathers of nestling ospreys (Pandion haliaetus) in Chesapeake and Delaware Bays

In 2000, 2001, and 2002, blood and feather samples were collected from 40–45-day-old nestling ospreys ( Pandion haliaetus ) from Chesapeake Bay and Delaware Bay and River. Concentrations of 18 metals, metalloids, and other elements were determined in these samples by inductively coupled plasma-mass spectroscopy, and Hg concentrations were measured by cold vapor atomic absorption spectroscopy. When compared to concurrent reference areas (South, West, and Rhode Rivers), mean As and Hg concentrations in blood were greater ( p < 0.05) in two of three Chesapeake Bay regions of concern (Baltimore Harbor [As: 1.18 vs. 0.548 μg/g dw], Anacostia River [Hg: 0.305 vs. 0.178 μg/g dw], and Elizabeth River [As: 0.876 vs. 0.663 μg/g dw; Hg: 0.260 vs. 0.180 μg/g dw]). Lead was detected more frequently in blood of nestlings from the highly industrialized Elizabeth River compared to the rural reference area. When compared to the concurrent reference area, mean Al, Ba, Hg, Mn, and Pb concentrations in feathers were substantially greater ( p < 0.05) in one or more Chesapeake regions of concern (Anacostia River [Al: 206 vs. 62.1 μg/g dw; Ba: 3.31 vs. 0.823 μg/g dw; Mn: 65.4 vs. 22.9 μg/g dw] and Elizabeth River [Al: 165 vs. 63.5 μg/g dw; Hg: 1.24 vs. 0.599 μg/g dw; Pb 1.47 vs. 0.543 μg/g dw]). When compared to the coastal Inland Bays reference area, feathers of nestlings from northern Delaware Bay and River had greater concentrations ( p < 0.05) of Ba (1.90 vs. 0.660 μg/g dw), Fe (258 vs. 109 μg/g dw), Mn (18.5 vs. 4.66 μg/g dw), Mo (0.130 vs. 0.040 μg/g dw), Pb (1.96 vs. 0.624 μg/g dw), and V (0.671 vs. 0.325 μg/g dw), presumably due to extensive metal-working and petroleum refinery activities. Concentrations of Hg in nestling feathers from Delaware were frequently greater than in the Chesapeake. The present findings and those of related reproductive studies suggest that concentrations of several heavy metals (e.g., Cd, Hg, Pb) in nestling blood and feathers from Chesapeake and Delaware Bays were below toxicity thresholds and do not seem to be affecting chick survival during the nestling period.

Delaware, Maryland, New Jersey, Virginia