Determination of the sulphur content of a lunar sample by neutron capture gamma-ray spectrometry

The technique of prompt neutron capture gamma-ray spectroscopy has been used to determine sulphur concentrations in extraterrestrial materials. In particular an effort was made to resolve reported discrepancies in the sulphur assays for the lunar rock sample 70215. While the validity of chemical analysis techniques are often influenced by the chemical form of the sulphur, particularly when in low concentration, the method used here is independent of such effects. The lunar and a bulk Allende meteorite sample were analyzed for sulphur, iron and silicon. The latter material, being well documented, was analyzed in order to verify the techniques of measurement and the subsequent methods of data reduction. Based upon our measurements and the acceptance of the silicon and iron content of the lunar sample the sulphur content was found to be 1741±112 ppm by weight.     

Determination of the sulphur content of geological samples by X-ray fluorescent analysis

Summary The sulphur content of ultramafic and basic rocks is determined by X-ray fluorescent analysis with pressed powder pellets. A commonly marked cellulose powder and wax are taken as diluent. Two analysing crystals, PET and graphite, are compared. The linear calibration curve reaches from 50 ppm to 1.0 weight-%, with a detection limit of 90 and 45 ppm, respectively. If the standard rock is of nearly the same matrix as the examined samples, no calculated matrix correction is necessary.

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Schwefelbestimmung in geologischen Proben durch Röntgenfluorescenz-Analyse

Zusammenfassung Eine Methode zur röntgenfluorescenzanalytischen Schwefelbestimmung an ultrabasischen und basischen Gesteinen wird beschrieben. Die Messung erfolgt an Preßtabletten mit handelsüblichem Cellulosepulver oder Wachs als Verdünnungsmittel. Zwei Analysatorkristalle, PET und Graphit, werden verglichen. Die lineare Eichkurve umfaßt den Konzentrationsbereich zwischen 50 ppm und 1 Gew.-% S. Die Nachweisgrenze liegt bei 90 bzw. 45 ppm, je nach verwendetem Kristall. Bei annähernd übereinstimmender Matrix von Standard- und Analysenprobe ist eine rechnerische Matrixkorrektur nicht erforderlich.

     

Determination of hydrogen in rock samples by neutron-induced prompt gamma-ray analysis

Prompt gamma-ray analysis was applied to determine hydrogen in geological samples. In order to obtain accurate values, blank values were estimated and subtracted. Samples were dried to constant weight in an oven. Helium gas was introduced into the sample box to purge the air containing moisture during the measurement. Hydrogen contents in some geochemical standard samples were determined and highly reproducible values were obtained.     

X射线荧光光谱法测定地质样品中的硫和氟

采用粉末压片制样-X射线荧光光谱法研究地质样品中硫(S)和氟(F)元素的快速测定方法。通过分级过筛实验优化确定样品粒度,探讨样品粒度对测定结果的影响,并进行实际样品和标准物质验证。结果显示,样品粒度为85μm时,经实际样品和标准物质验证,测定结果与化学值和标准认定值相符,且相对标准偏差(RSD)均小于2%。方法具有准确度高、检出限好、测试范围宽、简便快速等优点,能确保样品分析结果的准确性,实现了地质样品中S和F的快速测定。     

Determination of ash content in highly moistened coals by backscattered X-rays of109Cd

Theoretical and experimental results have shown that¹⁰⁹Cd X-rays are suitable for radioanalytical determinations of ash content in moistened coal. Errors due to variation of moisture are practically equal to zero, while those connected with the variations in iron and carbon content are acceptable.     

Determination of boron in Japanese geochemical reference samples by neutron-induced prompt gamma-ray analysis

Determination of ppm levels of B in 21 igneous and sedimentary rocks of the Japanese geochemical reference samples prepared by the Geological Survey of Japan (GSJ) has been performed by neutron-induced prompt γ-ray analysis (PGA) using cold and thermal guided neutron beams of the JRR-3M. Owing to the Doppler broadened γ-ray line of B 478 keV, many elements such as Na, Ni, Cl and so on showed spectral interference in the determination of B. The interference was corrected by computer fitting and a reference peak method. The analytical results obtained by the present method almost agreed with the GSJ values recommended in 1994 within the standard deviation of the recommended values. Sodium contents determined by the PGA in the reference rock samples are also reported.     

Neutron activation analysis of core and drill cutting samples from geothermal well drilling

Samples of sandstones and shales were analysed by instrumental neutron activation analysis for a total of 30 elements. Three irradiation and five counting periods wer employed. Solutions and National Bureau of Standards Reference Materials wer used for comparison. The samples were obtained from drill cuttings (with a few core samples) from drillings in the Salton Sea geothermal field of California. These determinations form part of a major study to elemental variation as a function of mineral variation as depth and temperature in the well vary. The overall goal is to examine mineral alteration and/or element migration under typical geothermal conditions. The techniques involve typical compromises between maximizing precision for individual element determinations and the amount of time and effort that can be expended, as it is desired to examine large numbers of samples. With the limitations imposed by the reactor flux ailable at the U. C. Irvine TRIGA reactor, the detectors available, and time factors, most precisions are acceptable for geological comparison purposes. Some additional measurements wer made by delayed-neutron counting methods to compare with uranium determinations made by conventional instrumental neutron activation analysis methods.     

Determination of the elemental sulphur content of minerals and ores

A new technique has been developed to determine trace quantities of elemental sulphur in minerals and ores. After separation from the sample by sublimation, the sulphur is determined spectrophotometrically in ethanol. Sulphide, sulphite, sulphate and thiosulphate do not interfere. The effect of the presence of xanthate or dixanthogen is discussed briefly.     

Determination of fluorine concentrations in soil samples using proton induced gamma-ray emission

A non-destructive, in situ current normalized particle induced gamma-ray emission methodology has been standardized for quantification of fluorine (F) in soil samples from Punjab state, India. The samples were irradiated using 4 MeV proton beam from the Folded Tandem Ion Accelerator at BARC, Mumbai. The gamma rays of energies 197 and 478 keV arising from ¹⁹F(p, p′γ)¹⁹F and ⁷Li(p, p′γ)⁷Li nuclear reactions were measured using high resolution gamma-ray spectrometry. The concentration of fluorine in soil samples was found to vary between 414 and 5,746 mg kg^?1.     

Determination of trace amounts of some metals in samples with high salt content by atomic absorption spectrometry after cobalt-diethyldithiocarbamate coprecipitation

A method for determination of trace amounts of Cu, Fe, Pb, Mn, Zn, Cd, Ni, Bi and Cr in aqueous solutions by flame atomic absorption spectrometry after coprecipitation by using a combination of sodium diethyldithiocarbamate as a chelating agent and cobalt as a carrier element was introduced. Different factors including amounts of reagents, pH of sample solution, standing time, sample volume for the precipitation and matrix effects were examined. Under selected conditions, the relative standard deviation of the combined method of sample treatment, coprecipitation and determination with flame AAS (n = 9) is generally about 3.5-6.9%; the limits of detection (3 s, n = 20) for the analytes were found to be between 4 and 64 microg 1(-1). The procedure was applied to the analysis of sea water and dialysis concentrate samples with quantitative recovery, > or =95%.     

Determination of selenium in biological samples by electrochemical preconcentration and atomic absorption spectrometry

Summary For the determination of selenium in biological materials the samples are digested with an HNO₃/H₂SO₄/ V₂O₅ or an HNO₃/HClO₄ mixture. Selenium is then electrolyzed onto a platinum wire, followed by atomic absorption spectrometry with simultaneous electrothermal and flame atomization. Results for the reference materials Bovine Liver and Albacore Tuna are reported (1–3±0.2 ppm Se).

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Selenbestimmung in biologischen Proben durch elektrochemische Anreicherung und Atomabsorptionsspektrometrie

Zusammenfassung Die Proben werden mit HNO₃/H₂SO₄/V₂O₅ oder HNO₃/HClO₄ aufgeschlossen; Se wird elektrolytisch auf einem Platindraht niedergeschlagen und durch AAS mit gleichzeitiger elektrothermischer und Flammen-Atomisierung bestimmt. Ergebnisse werden mitgeteilt für die Analyse von Standardreferenzmaterialien (Bovine Liver und Albacore Tuna, 1–3±0,2 ppm Se).

     

Determination of sulphur in fuel oils by absorption spectrometry of electrothermally generated carbon sulphide molecules

Molecular absorption spectra of CS are observed during the vaporization of crude and fuel oils in an electrothermal atomizer. The CS absorbance at 257.6 nm is used to determine the sulphur content of the oil, based on measurements in a conventional electrothermal atomic absorption spectrometer. The results for various fuel oils generally agree with those obtained by x-ray fluorescence spectrometry (ASTM D2622). The detection limit referred to the undiluted oil is 50 mg kg^?1, and the repeatability is 3% at the 250 mg kg^?1 level. Some oils exhibit uneven vaporization of sulphur species.     

Determination of chloride, nitrate, sulphate and total sulphur in environmental samples by single-column ion chromatography

The analytical performance characteristics of a single-column ion chromatography system are reported. The data were obtained by using conductivity detection as well as by an indirect ultraviolet technique. The method has been applied to the determination of Cl(-), NO(3)(-) and SO(4)(2-) in samples of rain, sewer water, and soil-pore water. Also described are two methods which allow ion Chromatographic analysis of CaS0(4)-extractable nitrate in soils, and total sulphur in soils, marine sediments and plant tissue.     

Correction by self-attenuation in gamma-ray spectrometry for environmental samples

Summary c/Herrera Oria s/n, 39011, Santan     

Determination of cadmium and lead in biological samples by three ultrasonic-based samples treatment procedures followed by electrothermal atomic absorption spectrometry

The development of 3 different ultrasonic-based sample treatment methods, ultrasonic probe-assisted acid extraction, ultrasonic-assisted acid slurry, and ultrasonic-assisted acid pseudodigestion is presented. These methods were compared for the determination of Cd and Pb by electrothermal atomic absorption spectrometry in biological samples (blood and scalp hair) and validated by using certified materials BCR 397 human hair and BCR 185R bovine liver. The sample amounts chosen to perform the analysis were 100 mg and 0.5 mL for solids (human hair and bovine liver) and blood samples, respectively. An acid digestion induced by microwave energy was used to obtain the total metal concentrations and for comparative purposes. The best results were obtained with the ultrasonic-assisted acid pseudodigestion, with which it was possible to perform accurate and precise determination of the Cd and Pb contents in 2 certified reference materials and biological samples of 50 normal males of ages 25-40 years. The precision of the methods, together with their efficiency, rapidity, low cost, and environmental acceptability, make them good alternatives for the determination of trace metals from biological samples. The precision of the methods for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level, and the relative standard deviations were lower than 10% (n=10) for all determinations.     

Determination of cadmium in biological and environmental samples by slurry electrothermal atomic absorption spectrometry

The retention of cadmium by the bacteria Escherichia coli and Pseudomonas putida was optimized in order to develop a rapid and selective preconcentration method for cadmium from biological and environmental samples prior to determination by electrothermal atomic absorption spectrometry. Living and lyophilized cells for both bacteria were used, but the method using dead cells shows better analytical capabilities. Cadmium from aqueous solutions is easily retained on the outer membrane of both bacteria in the pH range 4-10, although the selected working pHs for E. coli and P. putida were 5 and 9, respectively. Cadmium retained by the bacteria was dispersed in 3.5 M nitric acid and the slurry was introduced directly into the graphite tube. The best sensitivity and detection limit were obtained for E. coli (0.03 ng ml(-1) and 0.04 ng ml(-1) respectively, in the absence of any chemical modifier). A strong spectral interference from nickel chloride was found and methods to overcome it were developed. The proposed extraction procedure was tested by the determination of cadmium in different standard biological and environmental samples.     

Determination of mercury in environmental and biological samples by cold vapour atomic absorption spectrometry

A continuously operating monitoring method for total mercury at sub-ng/ml level in environmental and biological samples by cold vapour atomic-absorption spectrometry with NaBH₄ as a reductant was developed. The mercury vapour generator and absorption cell closed-end by quartz were used in this study. The detection limit (S/N = 3) and relative standard deviation of 12 determinations of 10 ng/ml Hg(II) were 0.11 ng/ml and 1.1%, respectively. The range of standard calibration curve was 0–50 ng/ml Hg, The proposed method was successfully applied to the completely continuous monitoring of total mercury in waste water, sediments and pork liver.     

Catalyst concentration distribution in fluidized bed by gamma-ray absorption

Summary The axial and radial distribution of the catalyst concentration, in the riser of an EMC - experimental cold model of a fluid catalytic cracking type unit, was measured by gamma-absorption. The solid concentration in the circulating fluidized bed was determined by measurements with a ²⁴¹Am gamma-source and a NaI(Tl) detector. The operation, instrumental measurements and data acquisition system of the cold unit were automated. The catalyst concentration measurements were carried out in static experiments and in the circulating fluidized bed. A calibration of the distribution concentration was made with experimental data from gas velocity and pressure drop along the riser that gave the best multi-regression model. A spatial resolution of 5.0 ^. 10^-3 m by scanning the riser and a catalyst density resolution of 5.0±0.8 kg/m³ were obtained. The axial catalyst concentration distribution, in the 5-13 kg/m ³ interval, showed a predicted pattern according to the literature. The radial distribution was in an annular configuration for this diluted catalyst concentration.