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Determination of color of turbid waters
A convenient procedure for determining the color of turbid waters, using the principle of precipitation of turbidity by the electrolyte calcium chloride, is described. Because the stable turbidity of many surface waters cannot be completely precipitated by conventional centrifuging alone, this procedure presents a means of flocculating the turbidity without affecting the true color of the water. In the determination of true color of turbid samples one of the most prevalent errors is caused by the reading of color on samples not completely free of turbidity. Pertinent data are presented on color and turbidity of waters as related to the principles involved in the determination of color.
Determination of thorium by fluorescent x-ray spectrometry
A fluorescent x-ray spectrographic method for the determination of thoria in rock samples uses thallium as an internal standard. Measurements are made with a two-channel spectrometer equipped with quartz (d = 1.817 A.) analyzing crystals. Particle-size effects are minimized by grinding the sample components with a mixture of silicon carbide and aluminum and then briquetting. Analyses of 17 samples showed that for the 16 samples containing over 0.7% thoria the average error, based on chemical results, is 4.7% and the maximum error, 9.5%. Because of limitations of instrumentation, 0.2% thoria is considered the lower limit of detection. An analysis can be made in about an hour.
Aluminum powder as a binder in sample preparation for X-ray spectrometry
[No abstract available]
Field method for determination of traces of arsenic in soils: Confined spot procedure using a modified Gutzeit apparatus
[No abstract available]
Method for determination of small amounts of rare earths and thorium in phosphate rocks
In laboratory investigations, interest developed in the possible rare-earth content of phosphate samples from Florida and the northwestern United States. Because of the difficulty of making chemical determinations of traces of individual rare earths, a combined chemical-spectrographic method was investigated. After removal of iron by the extraction of the chloride with ether, the rare earths and thorium are concentrated by double oxalate precipitation, using calcium as a carrier. The rare earths are freed from calcium by an ammonium hydroxide precipitation with a fixed amount of aluminum as a carrier. The aluminum also serves as an internal standard in the final spectrographic analysis. The method will determine from 0.02 to 2 mg. of each rare earth with an error no greater than 10%. The investigation has resulted in a fairly rapid and precise procedure, involving no special spectrographic setup. The method could be applied to other types of geologic materials with the same expected accuracy.
Determination of traces of cobalt in soils: A field method
The growing use of geochemical prospecting methods in the search for ore deposits has led to the development of a field method for the determination of cobalt in soils. The determination is based on the fact that cobalt reacts with 2-nitroso-1-naphthol to yield a pink compound that is soluble in carbon tetrachloride. The carbon tetrachloride extract is shaken with dilute cyanide to complex interfering elements and to remove excess reagent. The cobalt content is estimated by comparing the pink color in the carbon tetrachloride with a standard series prepared from standard solutions. The cobalt 2-nitroso-1-naphtholate system in carbon tetrachloride follows Beer's law. As little as 1 p.p.m. can be determined in a 0.1-gram sample. The method is simple and fast and requires only simple equipment. More than 40 samples can be analyzed per man-day with an accuracy within 30% or better.
Determination of lithium in rocks: Fluorometric method
The gravimetric method in general use for the determination of lithium is tedious, and the final weighed product often contains other alkali metals. A fluorometric method was developed to shorten the time required for the analysis and to assure that the final determination is for lithium alone. This procedure is based on the complex formed between lithium and 8-hydroxyquinoline. The fluorescence is developed in a slightly alkaline solution of 95% alcohol and measurement is made on a photoelectric fluorometer. Separation from the ore is carried out by the wet method or by the distillation procedure. Sodium and potassium are removed by alcohol and ether, but complete separation is not necessary. Comparison of analyzed samples shows excellent agreement with spectrographic and gravimetric methods. The fluorometric method is more rapid than the gravimetric and produces more conclusive results. Another useful application is in the preparation of standard lithium solutions from reagent quality salts when a known standard is available. In this case no separations are necessary.
Determination of molybenum in soils and rocks: A geochemical semimicro field method
Reconnaissance work in geochemical prospecting requires a simple, rapid, and moderately accurate method for the determination of small amounts of molybdenum in soils and rocks. The useful range of the suggested procedure is from 1 to 32 p.p.m. of molybdenum, but the upper limit can be extended. Duplicate determinations on eight soil samples containing less than 10 p.p.m. of molybdenum agree within 1 p.p.m., and a comparison of field results with those obtained by a conventional laboratory procedure shows that the method is sufficiently accurate for use in geochemical prospecting. The time required for analysis and the quantities of reagents needed have been decreased to provide essentially a "test tube" method for the determination of molybdenum in soils and rocks. With a minimum amount of skill, one analyst can make 30 molybdenum determinations in an 8-hour day.
Fluorometric determination of zirconium in minerals
The increasing use of zirconium in alloys and in the ceramics industry has created renewed interest in methods for its determination. It is a common constituent of many minerals, but is usually present in very small amounts. Published methods tend to be tedious, time-consuming, and uncertain as to accuracy. A new fluorometric procedure, which overcomes these objections to a large extent, is based on the blue fluorescence given by zirconium and flavonol in sulfuric acid solution. Hafnium is the only element that interferes. The sample is fused with borax glass and sodium carbonate and extracted with water. The residue is dissolved in sulfuric acid, made alkaline with sodium hydroxide to separate aluminum, and filtered. The precipitate is dissolved in sulfuric acid and electrolysed in a Melaven cell to remove iron. Flavonol is then added and the fluorescence intensity is measured with a photo-fluorometer. Analysis of seven standard mineral samples shows excellent results. The method is especially useful for minerals containing less than 0.25% zirconium oxide.
Geochemical field method for determination of nickel in plants
The use of biogeochemical data in prospecting for nickel emphasizes the need for a simple, moderately accurate field method for the determination of nickel in plants. In order to follow leads provided by plants of unusual nickel content without loss of time, the plants should be analyzed and the results given to the field geologist promptly. The method reported in this paper was developed to meet this need. Speed is acquired by elimination of the customary drying and controlled ashing; the fresh vegetation is ashed in an open dish over a gasoline stove. The ash is put into solution with hydrochloric acid and the solution buffered. A chromograph is used to make a confined spot with an aliquot of the ash solution on dimethylglyoxime reagent paper. As little as 0.025% nickel in plant ash can be determined. With a simple modification, 0.003% can be detected. Data are given comparing the results obtained by an accepted laboratory procedure. Results by the field method are within 30% of the laboratory values. The field method for nickel in plants meets the requirements of biogeochemical prospecting with respect to accuracy, simplicity, speed, and ease of performance in the field. With experience, an analyst can make 30 determinations in an 8-hour work day in the field.
Automatic micromuffle for determination of ash in carbonaceous material
No abstract available.
Redox chemistry and natural organic matter (NOM): Geochemists' dream, analytical chemists' nightmare
Natural organic matter (NOM) is an inherently complex mixture of polyfunctional organic molecules. Because of their universality and chemical reversibility, oxidation/reductions (redox) reactions of NOM have an especially interesting and important role in geochemistry. Variabilities in NOM composition and chemistry make studies of its redox chemistry particularly challenging, and details of NOM-mediated redox reactions are only partially understood. This is in large part due to the analytical difficulties associated with NOM characterization and the wide range of reagents and experimental systems used to study NOM redox reactions. This chapter provides a summary of the ongoing efforts to provide a coherent comprehension of aqueous redox chemistry involving NOM and of techniques for chemical characterization of NOM. It also describes some attempts to confirm the roles of different structural moieties in redox reactions. In addition, we discuss some of the operational parameters used to describe NOM redox capacities and redox states, and describe nomenclature of NOM redox chemistry. Several relatively facile experimental methods applicable to predictions of the NOM redox activity and redox states of NOM samples are discussed, with special attention to the proposed use of fluorescence spectroscopy to predict relevant redox characteristics of NOM samples.
Influence of sediment chemistry and sediment toxicity on macroinvertebrate communities across 99 wadable streams of the Midwestern USA
Simultaneous assessment of sediment chemistry, sediment toxicity, and macroinvertebrate communities can provide multiple lines of evidence when investigating relations between sediment contaminants and ecological degradation. These three measures were evaluated at 99 wadable stream sites across 11 states in the Midwestern United States during the summer of 2013 to assess sediment pollution across a large agricultural landscape. This evaluation considers an extensive suite of sediment chemistry totaling 274 analytes (polycyclic aromatic hydrocarbons, organochlorine compounds, polychlorinated biphenyls, polybrominated diphenyl ethers, trace elements, and current-use pesticides) and a mixture assessment based on the ratios of detected compounds to available effects-based benchmarks. The sediments were tested for toxicity with the amphipod Hyalella azteca (28-d exposure), the midge Chironomus dilutus (10-d), and, at a few sites, with the freshwater mussel Lampsilis siliquoidea (28-d). Sediment concentrations, normalized to organic carbon content, infrequently exceeded benchmarks for aquatic health, which was generally consistent with low rates of observed toxicity. However, the benchmark-based mixture score and the pyrethroid insecticide bifenthrin were significantly related to observed sediment toxicity. The sediment mixture score and bifenthrin were also significant predictors of the upper limits of several univariate measures of the macroinvertebrate community (EPT percent, MMI (Macroinvertebrate Multimetric Index) Score, Ephemeroptera and Trichoptera richness) using quantile regression. Multivariate pattern matching (Mantel-like tests) of macroinvertebrate species per site to identified contaminant metrics and sediment toxicity also indicate that the sediment mixture score and bifenthrin have weak, albeit significant, influence on the observed invertebrate community composition. Together, these three lines of evidence (toxicity tests, univariate metrics, and multivariate community analysis) suggest that elevated contaminant concentrations in sediments, in particular bifenthrin, is limiting macroinvertebrate communities in several of these Midwest streams.
Effects of season, location, species, and sex on hematologic and plasma biochemical values and body mass in free-ranging Grebes (Aechmophorus species)
The effects of season, location, species, and sex on body weight and a comprehensive array of blood chemistry and hematology analytes were compared for free-ranging western ( Aechmophorus occidentalis ) and Clark's ( Aechmophorus clarkii ) grebes. Birds (n = 56) were collected from Puget Sound, WA, and Monterey Bay and San Francisco Bay, CA, from February 2007 to March 2011. The data supported generalization of observed ranges for most analytes across Aechmophoru s grebe metapopulations wintering on the Pacific coast. Notable seasonal and location effects were observed for packed cell volume (winter 6% greater than fall; winter California [CA] 5% greater than Washington [WA]), total white blood cell count (CA 3.57 × 10 3 cells/µL greater than WA), heterophils (WA 10% greater than CA), lymphocytes (winter 19% greater than fall), heterophil to lymphocyte ratio (fall 5.7 greater than winter), basophils (CA greater than WA), plasma protein (WA about 10 g/L [1.0 g/dL] greater than CA), plasma protein to fibrinogen ratio (winter about 15 greater than fall), potassium (CA 2 mmol/L greater than WA), and liver enzymes (alanine aminotransferase, aspartate aminotransferase, lactate dehydrogenase: WA greater than CA). Within California, season had a greater effect on body mass than sex (mean winter weights about 200 g greater than fall), whereas within a season, males weighed only about 80 g more than females, on average. These data give biologists and veterinarians quantitative reference values to better assess health at the individual and metapopulation level.