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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↗

Compositional data for Bengal delta sediment collected from boreholes at Srirampur, Kachua, Bangladesh

Processes active within sediment of the Bengal delta have attracted world concern because of the locally high content of arsenic dissolved in ground water drawn from that sediment. Sediment samples were collected from two boreholes in Srirampur village, Kachua upazila, Chandphur district, Bangladesh, to investigate the processes contributing to arsenic contamination. The samples were mineralogically and chemically analyzed to determine compositional variations related to the arsenic content of the sediment. Mineralogy of the sediments was determined using powder X-ray diffraction. Bulk chemical composition was measured by Combustion, Inductively Coupled Plasma Atomic Emission Spectroscopy, Energy Dispersive X-ray Fluorescence, and Hydride Generation Atomic Absorption Spectrophotometry. Solutions produced by four chemical extractions-0.1 molar strontium chloride, 0.5 normal hydrochloric acid, titanium(III)-EDTA, and a solution of hydrogen peroxide and hydrochloric acid-were analyzed to evaluate the chemical reactivity of the sediment with an emphasis on arsenic residence. Acid-volatile sulfide, acid-soluble sulfate, and reducible sulfide were also measured. Sediment sampled at Srirampur is typically unlithified, gray, micaceous, feldspathic, arenaceous silt and sand. Arsenic content of the sediment ranges from <1 to 210 ppm, with the highest contents measured in sediment collected at a depth of 320 meters. Samples with high arsenic contents typically contain high concentrations of sulfur. The greatest amount of arsenic was extracted using the oxidative hydrogen peroxide and hydrochloric acid extraction solution. The extraction results are consistent with the apparent association of arsenic in sulfur in the bulk chemical analyses. Pyrite is typically the most abundant form of sulfur in the sediment and is dissolved by the oxidative extraction.

Open-File Report↗

Compositional Data for Bengal Delta Sediment Collected from a Borehole at Rajoir, Bangladesh

Processes active within sediment of the Bengal basin have attracted world concern because of the locally high content of arsenic dissolved in ground water drawn from that sediment. Sediment samples were collected from a borehole in the town of Rajoir, Rajoir upazila, Madaripur district, Bangladesh, to investigate the processes contributing to arsenic contamination. The samples were mineralogically and chemically analyzed to determine compositional variations related to the arsenic content of the sediment. Mineralogy of the sediment was determined using powder X-ray diffraction. Bulk chemical composition was measured by Combustion; Inductively Coupled Plasma Atomic Emission Spectroscopy; Energy Dispersive X-ray Fluorescence; and Hydride Generation Atomic Absorption Spectrophotometry. Sediment was treated with 0.5 N HCl and resulting solutions were analyzed, primarily to evaluate the abundance and oxidation state of acid-soluble iron. Acid-volatile sulfide, acid-soluble sulfate, and reducible sulfide were also measured on a few samples. Sediment sampled at Rajoir is typically unlithified, gray, micaceous, feldspathic arenaceous sand with a few silt and clay layers. Arsenic content of the sediment ranges from 0.6 to 21 ppm with a median of 1.2 ppm.

Open-File Report↗

Geochemical analysis of soils and sediments, Coeur d'Alene drainage basin, Idaho: sampling, analytical methods, and results

This report presents the locations, descriptions, analytical procedures used, and an inter-lab comparison of over 1100 geochemical analyses of samples of soil and sediment in and downstream of a major lead-zinc-silver mining district in the Coeur d'Alene (CdA) drainage basin of northern Idaho. The samples fall in 3 broad categories: (1) samples from vertical profiles of floodplain soils in the valley of the main stem of the CdA River (767 samples) and of the South Fork of the CdA River (38 samples), (2) size fractionated surficial samples of sediment bedload within the channel of the South Fork of the CdA River (68 samples), and (3) samples from vertical profiles of sediment bedload within the channel of the main stem of the CdA River (260 samples). Five different laboratories contributed geochemical data for this report. Four of the five laboratories employed analytical methods that require sample dissolution prior to analysis; one laboratory (US Geological Survey) used analytical instrumentation (energy dispersive x-ray fluorescence [EDXRF]) that is applied to pulverized samples. Some dissolution procedures use four acids (hydrochloric, nitric, perchloric, and hydrofluoric; Eastern Washington University [EWU] Geochemical Laboratory and XRAL Laboratories, Inc.), others use two acids (nitric acid and aqua regia; CHEMEX Labs, Inc.), and some use only concentrated nitric acid (ACZ Laboratories, Inc.). Most analyses of dissolved samples were done by Inductively Coupled Plasma - Atomic Emission Spectroscopy (ICP-AES) or by ICP - MS (Mass Spectroscopy). Some analyses for Ag and K were done by Flame Atomic Absorption (FAA). Inter-laboratory comparisons are made for 6 elements: lead (Pb), zinc (Zn), iron (Fe), manganese (Mn), arsenic (As), and cadmium (Cd). In general inter-laboratory correlations are better for samples within the compositional range of the Standard Reference Materials (SRMs) from the National Institute of Standards and Technology (NIST). Analyses by EWU are the most accurate relative to the NIST standards (mean recoveries within 1% for Pb, Fe, Mn, and As, 3% for Zn and 5% for Cd) and are the most precise (within 7% of the mean at the 95% confidence interval). USGS-EDXRF is similarly accurate for Pb and Zn. XRAL and ACZ are relatively accurate for Pb (within 5-8% of certified NIST values), but were considerably less accurate for the other 5 elements of concern (10-25% of NIST values). However, analyses of sample splits by more than one laboratory reveal that, for some elements, XRAL (Pb, Mn, Cd) and ACZ (Pb, Mn, Zn, Fe) analyses were comparable to EWU analyses of the same samples (when values are within the range of NIST SRMs). These results suggest that, for some elements, XRAL and ACZ dissolutions are more effective on the matrix of the CdA samples than on the matrix of the NIST samples (obtained from soils around Butte, Montana). Splits of CdA samples analyzed by CHEMEX were the least accurate, yielding values 10-25% less than those of EWU.

Idaho↗

A rapid, partial leach and organic separation for the sensitive determination of Ag, Bi, Cd, Cu, Mo, Pb, Sb, and Zn in surface geologic materials by flame atomic absorption

A solution of dilute hydrochloric acid, ascorbic acid, and potassium iodide has been found to dissolve weakly bound metals in soils, stream sediments, and oxidized rocks. Silver, Bi, Cd, Cu, Mo, Pb, Sb, and Zn are selectively extracted from this solution by a mixture of Aliquat 336 (tricaprylyl methyl ammonium chloride) and MIBK (methyl isobutyl ketone). Because potentially interfering major and minor elements do not extract, the organic separation allows interference-free determinations of Ag and Cd to the 0.05 ppm level, Mo, Cu, and Zn to 0.5 ppm, and Bi, Pb, and Sb to 1 ppm in the sample using flame atomic absorption spectroscopy. The analytical absorbance values of the organic solution used in the proposed method are generally enhanced more than threefold as compared to aqueous solutions, due to more efficient atomization and burning characteristics. The leaching and extraction procedures are extremely rapid; as many as 100 samples may be analyzed per day, yielding 800 determinations, and the technique is adaptable to field use. The proposed method was compared to total digestion methods for geochemical reference samples as well as soils and stream sediments from mineralized and unmineralized areas. The partial leach showed better anomaly contrasts than did total digestions. Because the proposed method is very rapid and is sensitive to pathfinder elements for several types of ore deposits, it should be useful for reconnaissance surveys for concealed deposits.

Journal of Geochemical Exploration↗

A comparison of geochemical exploration techniques and sample media within accretionary continental margins: an example from the Pacific Border Ranges, Southern Alaska, U.S.A.

The Pacific Border Ranges of the southern Alaskan Cordillera are composed of a number of allochthonous tectonostratigraphic terranes. Within these terranes are widespread volcanogenic, massive sulfide deposits in and adjacent to portions of accreted ophiolite complexes, bands and disseminations of chromite in accreted island-arc ultramafic rocks, and epigenetic, gold-bearing quartz veins in metamorphosed turbidite sequences. A geochemical pilot study was undertaken to determine the most efficient exploration strategy for locating these types of mineral deposits within the Pacific Border Ranges and other typical convergent continental margin environments. High-density sediment sampling was carried out in first- and second-order stream channels surrounding typical gold, chromite and massive sulfide occurrences. At each site, a stream-sediment and a panned-concentrate sample were collected. In the laboratory, the stream sediments were sieved into coarse-sand, fine- to medium-sand, and silt- to clay-size fractions prior to analysis. One split of the panned concentrates was retained for analysis; a second split was further concentrated by gravity separation in heavy liquids and then divided into magnetic, weakly magnetic and nonmagnetic fractions for analysis. A number of different techniques including atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry and semi-quantitative emission spectrography were used to analyze the various sample media. Comparison of the various types of sample media shows that in this tectonic environment it is most efficient to include a silt- to clay-size sediment fraction and a panned-concentrate sample. Even with the relatively low detection limits for many elements by plasma spectrometry and atomic absorption spectrometry, anomalies reflecting the presence of gold veins could not be identified in any of the stream-sediment fractions. Unseparated panned-concentrate samples should be analyzed by emission spectroscopy and atomic absorption spectrometry for Ag and Au. If, however, magnetic and nonmagnetic concentrate fractions are used in a reconnaissance program, semiquantitative emission spectrography is adequate for all analytical work.

Journal of Geochemical Exploration↗

Chemical composition of the hydrothermal fluids responsible for the lead-zinc deposits at Providencia, Zacatecas, Mexico

The chemical composition of 22 samples of primary fluid inclusions in quartz, calcite, and sphalerite from Providencia, Mexico, has been determined. Samples were prepared, crushed, and leached as described by Roedder et al. (1963). Cation analyses of leachates were made by atomic absorption spectroscopy, and the anions were analyzed by a special X-ray fluorescence technique. The Na, K, Ca, and C1 concentrations show a considerable range that reflects the widespread salinity variations in the hydrothermal fluids observed by Sawkins (1964). The K/Na atomic ratios of most samples range from 0.18 to 0.43 and the ratios tend to increase with the salinity of the inclusions. The temperatures indicated by the K/Na ratios from the published curves of K/Na ratios vs. temperature are mostly at least 100 ø C greater than corresponding filling temperatures. The Ca/Na atomic ratios of inclusions in sphalerite range from 0.12 to 0.61. The K/Na and Ca/Na data agree well with previous δO¹⁸ data (Rye, 1966; Rye and O'Neil. 1968) which indicate that the hydrothermal fluids were derived from the magma related to the Providencia granodiorite stock and that the fluids reacted only slightly with the crystalline stock during the late phases of ore deposition. The data also indicate that the salinity variations in the hydrothermal fluids probably occurred at the source of the fluids and may have resulted from boiling in the magma chamber. Mg concentrations are generally no more than a few hundred parts per million. Most of the Mg in the hydrothermal fluids was evidently removed during the formation of calcium-magnesium silicates in the lower levels of the ore pipes. Mg/Ca atomic ratios are generally less than 0.08 and are consistent with the paucity of dolomite in the area. Zn and Cu concentrations in water leaches of inclusions in calcite are generally less than 50 ppm. Maximum base-metal concentrations from water leaches of two samples of inclusions in quartz are 890 ppm Zn and 530 ppm Cu. Chloride is the major anion in the fluids, and C1 concentrations vary with corresponding cation concentrations. With two exceptions, sulfur concentrations of the inclusions in calcite and quartz, analyzed as SO₄, are below the level of detection

Zacatecas↗

Improving ChemCam LIBS long-distance elemental compositions using empirical abundance trends

The ChemCam instrument on the Curiosity rover provides chemical compositions of Martian rocks and soils using remote laser-induced breakdown spectroscopy (LIBS). The elemental calibration is stable as a function of distance for Ti, Fe, Mg, and Ca. The calibration shows small, systematically increasing abundance trends as a function of distance for Al, Na, K, and to some extent, Si. The distance effect is known to be due to a dependence with distance on the relative strengths of atomic transition lines. Emission lines representing transitions from relatively low energy levels remain intense at longer distances while emission lines representing transitions from higher energy levels decrease in intensity more rapidly as a function of distance. The multivariate algorithms used to determine elemental compositions rely on a large number of emission lines in many cases, so rather than trying to correct all emission lines, a study was made of the predicted compositions as a function of distance, in order to determine an empirical correction. Abundance trends can be well approximated by a linear trend with distance within the ranges of abundances and distances observed up to ~6 m. Data from 11 distinct geological members and data groups of the Murray formation in Gale crater, Mars, were used to form the model, selecting the members and data groups yielding the best statistics. The model was tested using data from several targets observed from two different distances, and using data from the Kimberley formation, the composition of which is significantly different from the Murray formation, showing that the model works on other compositions beyond those used to build the model. For long-distance observations up to ~6 m, corrections can be made back to an equivalent composition at the median distance of ChemCam observations (2.6 m). The model has been validated up to 6.2 m, although ChemCam is able to observe bedrock targets to >7 m, and iron meteorites to distances of >9 m.

Spectrochimica Acta Part B: Atomic Spectroscopy↗

Methods for analysis of selected metals in water by atomic absorption

This manual describes atomic-absorption-spectroscopy methods for determining calcium, copper, lithium, magnesium, manganese, potassium, sodium, strontium and zinc in atmospheric precipitation, fresh waters, and brines. The procedures are intended to be used by water quality laboratories of the Water Resources Division of the U.S. Geological Survey. Detailed procedures, calculations, and methods for the preparation of reagents are given for each element along with data on accuracy, precision, and sensitivity. Other topics discussed briefly are the principle of atomic absorption, instrumentation used, and special analytical techniques.

Water Supply Paper↗

Finalization of the Confocal Laser Scanning Microscopy (CLSM) working group

A working group in Commission II to investigate applications of confocal laser scanning microscopy (CLSM) for organic petrology investigations has finalized with publication of the manuscript “Characterization of bituminite in Kimmeridge Clay by confocal laser scanning and atomic force microscopy” in the International Journal of Coal Geology. The manuscript is available via Open Access from https://doi.org/10.1016/j.coal.2022.103927 and also from the Commission II working group (WG) webpage https://www.iccop.org/workinggroup/confocal-laser-scanning-microscopy-clsm/. A report detailing the full history and results from the WG also is available from the Commission II WG webpage. The working group investigated the application of CLSM to an organic-rich (44 wt.% TOC), thermally immature sample (VRo 0.42%) of the Kimmeridge Clay Formation. CLSM imaging and spectroscopy and atomic force microscopy (AFM) were used to characterize bituminite.

ICCP News↗

Improved accuracy in quantitative laser-induced breakdown spectroscopy using sub-models

Accurate quantitative analysis of diverse geologic materials is one of the primary challenges faced by the Laser-Induced Breakdown Spectroscopy (LIBS)-based ChemCam instrument on the Mars Science Laboratory (MSL) rover. The SuperCam instrument on the Mars 2020 rover, as well as other LIBS instruments developed for geochemical analysis on Earth or other planets, will face the same challenge. Consequently, part of the ChemCam science team has focused on the development of improved multivariate analysis calibrations methods. Developing a single regression model capable of accurately determining the composition of very different target materials is difficult because the response of an element’s emission lines in LIBS spectra can vary with the concentration of other elements. We demonstrate a conceptually simple “sub-model” method for improving the accuracy of quantitative LIBS analysis of diverse target materials. The method is based on training several regression models on sets of targets with limited composition ranges and then “blending” these “sub-models” into a single final result. Tests of the sub-model method show improvement in test set root mean squared error of prediction (RMSEP) for almost all cases. The sub-model method, using partial least squares regression (PLS), is being used as part of the current ChemCam quantitative calibration, but the sub-model method is applicable to any multivariate regression method and may yield similar improvements.

Spectrochimica Acta Part B: Atomic Spectroscopy↗

Recalibration of the Mars Science Laboratory ChemCam instrument with an expanded geochemical database

The ChemCam Laser-Induced Breakdown Spectroscopy (LIBS) instrument onboard the Mars Science Laboratory (MSL) rover Curiosity has obtained > 300,000 spectra of rock and soil analysis targets since landing at Gale Crater in 2012, and the spectra represent perhaps the largest publicly-available LIBS datasets. The compositions of the major elements, reported as oxides (SiO 2 , TiO 2 , Al 2 O 3 , FeO T , MgO, CaO, Na 2 O, K 2 O), have been re-calibrated using a laboratory LIBS instrument, Mars-like atmospheric conditions, and a much larger set of standards (408) that span a wider compositional range than previously employed. The new calibration uses a combination of partial least squares (PLS1) and Independent Component Analysis (ICA) algorithms, together with a calibration transfer matrix to minimize differences between the conditions under which the standards were analyzed in the laboratory and the conditions on Mars. While the previous model provided good results in the compositional range near the average Mars surface composition, the new model fits the extreme compositions far better. Examples are given for plagioclase feldspars, where silicon was significantly over-estimated by the previous model, and for calcium-sulfate veins, where silicon compositions near zero were inaccurate. The uncertainties of major element abundances are described as a function of the abundances, and are overall significantly lower than the previous model, enabling important new geochemical interpretations of the data.

Spectrochimica Acta Part B: Atomic Spectroscopy↗

Pre-flight calibration and initial data processing for the ChemCam laser-induced breakdown spectroscopy instrument on the Mars Science Laboratory rover

The ChemCam instrument package on the Mars Science Laboratory rover, Curiosity, is the first planetary science instrument to employ laser-induced breakdown spectroscopy (LIBS) to determine the compositions of geological samples on another planet. Pre-processing of the spectra involves subtracting the ambient light background, removing noise, removing the electron continuum, calibrating for the wavelength, correcting for the variable distance to the target, and applying a wavelength-dependent correction for the instrument response. Further processing of the data uses multivariate and univariate comparisons with a LIBS spectral library developed prior to launch as well as comparisons with several on-board standards post-landing. The level-2 data products include semi-quantitative abundances derived from partial least squares regression. A LIBS spectral library was developed using 69 rock standards in the form of pressed powder disks, glasses, and ceramics to minimize heterogeneity on the scale of the observation (350–550 μm dia.). The standards covered typical compositional ranges of igneous materials and also included sulfates, carbonates, and phyllosilicates. The provenance and elemental and mineralogical compositions of these standards are described. Spectral characteristics of this data set are presented, including the size distribution and integrated irradiances of the plasmas, and a proxy for plasma temperature as a function of distance from the instrument. Two laboratory-based clones of ChemCam reside in Los Alamos and Toulouse for the purpose of adding new spectra to the database as the need arises. Sensitivity to differences in wavelength correlation to spectral channels and spectral resolution has been investigated, indicating that spectral registration needs to be within half a pixel and resolution needs to match within 1.5 to 2.6 pixels. Absolute errors are tabulated for derived compositions of each major element in each standard using PLS regression. Sources of errors are investigated and discussed, and methods for improving the analytical accuracy of compositions derived from ChemCam spectra are discussed.

Spectrochimica Acta Part B: Atomic Spectroscopy↗

Chemical and textural controls on phosphorus mobility in drylands of southeastern Utah

We investigated several forms of phosphorus (P) in dryland soils to examine the chemical and textural controls on P stabilization on a diverse set of substrates. We examined three P fractions including labile, moderately labile, and occluded as determined by a modified Hedley fractionation technique. The P fractions were compared to texture measurements and total elemental concentrations determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Labile P related to the absence of materials involved in P sorption. Moderately labile P was most strongly associated with high total Al & Fe content that we interpret to represent oxides and 1:1 clay minerals. The occluded P fraction was strongly associated with low total Al & Fe environments and interpreted to represent 2:1 clay minerals where ligand exchange tightly sequesters P. The results indicate that the controls on P fraction distribution are initially closely tied to the chemical and physical properties of the bedrock units that contribute to soil formation. Further, these results suggest that the progression of stabilized P forms in dryland areas differs from the progression observed in mesic environments. Soil development in dryland settings, such as the formation of pedogenic carbonates, may lead to differing controls on P availability and the proportional size of the moderately labile fraction.

Utah↗

The group separation of the rare-earth elements and yttrium from geologic materials by cation-exchange chromatography

Demand is increasing for the determination of the rare-earth elements (REE) and yttrium in geologic materials. Due to their low natural abundance in many materials and the interferences that occur in many methods of determination, a separation procedure utilizing gradient strong-acid cation-exchange chromatography is often used to preconcentrate and isolate these elements from the host-rock matrix. Two separate gradient strong-acid cation-exchange procedures were characterized and the major elements as well as those elements thought to provide the greatest interference for the determination of the REE in geologic materials were tested for separation from the REE. Simultaneous inductively coupled argon plasma-atomic emission spectroscopy (ICAP-AES) measurements were used to construct the chromatograms for the elution studies, allowing the elution patterns of all the elements of interest to be determined in a single fraction of eluent. As a rock matrix, U.S. Geological Survey standard reference BCR-1 basalt was digested using both an acid decomposition procedure and a lithium metaborate fusion. Hydrochloric and nitric acids were tested as eluents and chromatograms were plotted using the ICAP-AES data; and we observed substantial differences in the elution patterns of the REE and as well as in the solution patterns of Ba, Ca, Fe and Sr. The nitric acid elution required substantially less eluent to elute the REE and Y as a group when compared to the hydrochloric acid elution, and provided a clearer separation of the REE from interfering and matrix elements. ?? 1984.

Chemical Geology↗

Extraction of vanadium into isobutyl methyl ketone

Because of its advantages in atomic-absorption spectroscopy, isobutyl methyl ketone was chosen as organic solvent for an extraction study on vanadium. Of eight chelating agents which were evaluated for completeness of extraction, ease of use, working pH range, and freedom from interference, cupferron was judged best.

Talanta↗

Separation and preconcentration of the rare-earth elements and yttrium from geological materials by ion-exchange and sequential acid elution

The abundance of rare-earth elements (REE) and yttrium in geological materials is generally low, and most samples contain elements that interfere in the determination of the REE and Y, so a separation and/or preconcentration step is often necessary. This is often achieved by ion-exchange chromatography with either nitric or hydrochloric acid. It is advantageous, however, to use both acids sequentially. The final solution thus obtained contains only the REE and Y, with minor amounts of Al, Ba, Ca, Sc, Sr and Ti. Elements that potentially interfere, such as Be, Co, Cr, Fe, Mn, Th, U, V and Zr, are virtually eliminated. Inductively-coupled argon plasma atomic-emission spectroscopy can then be used for a final precise and accurate measurement. The method can also be used with other instrumental methods of analysis.

Talanta↗

Emission spectrographic determination of volatile trace elements in geologic materials by a carrier distillation technique

Trace levels of chalcophile elements that form volatile sulfide minerals are determined in stream sediments and in the nonmagnetic fraction of a heavy-mineral concentrate of stream sediments by a carrier distillation emission spectrographic method. Photographically recorded spectra of samples are visually compared with those of synthetic standards for the two sample types. Rock and soil samples may also be analyzed by comparison with the stream-sediment standards. A gallium oxide spectrochemical carrier/buffer enhances the early emission of the volatile elements. Detection limits in parts per million attained are: Sb 5, As 20, Bi 0.1, Cd 1, Cu 1, Pb 2, Ag 0.1, Zn 2, and Sn 0.1. A comparison with other methods of analysis, total-burn emission and atomic absorption spectroscopy, shows good correlation for standard reference for materials and samples from a variety of geologic terranes.

Journal of Geochemical Exploration↗