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H. J. Rose

Publications and source records attributed to H. J. Rose.

12 recordsLinked to original sources
USGS2002

The detection of sulphur in contamination spots in electron probe X-ray microanalysis

Sulphur has been identified as one of the elements present in the contamination spot which forms under the electron beam in the microprobe. The presence of the sulphur results in a rapid change in intensity measurements causing a loss of observed intensity for elements other than sulphur. The source of sulphur has been traced at least in part to the Apiezon B diffusion pump oil. A comparative X-ray fluorescence study of the Apiezon B and Octoil diffusion pump oils showed substantial amounts of sulphur in the Apiezon B. The Octoil was relatively free of sulphur.

British Journal of Applied Physics↗
USGS1976

Preliminary results from the Viking x-ray fluorescence experiment: The first sample from Chryse Planitia, Mars

Iron, calcium, aluminum, silicon, and sulfur are major elements in the first surface sample of Mars that has been analyzed by the Viking x-ray fluorescence spectrometer. Titanium is present in minor quantities. This is consistent with the sample being a mixture of fine silicate and oxide mineral grains, with a significant proportion of sulfates, possibly hydrated. Ferric oxide is regarded as the red pigmenting agent on the martian surface, but if it coats silicate grains, the coatings must be very thin (≤ 2 micrometers) or discontinuous. A high abundance of Fe, relatively low abundances of Al, Rb, Sr, and Zr, and a high Ca/K ratio are distinctive features of the spectra. Preliminary determinations indicate the following abundances (as percentages by weight): Fe, 14 ± 2; Ti < 1; S, 2 to 5; the Ca/K ratio by weight is greater than 5.

Science↗
USGS1973

Inorganic chemical investigation by x-ray fluorescence analysis: The Viking Mars Lander

The inorganic chemical investigation added in August 1972 to the Viking Lander scientific package will utilize an energy-dispersive X-ray fluorescence spectrometer in which four sealed, gas-filled proportional counters will detect X-rays emitted from samples of the Martian surface materials irradiated by X-rays from radioisotope sources ( 55 Fe and 109 Cd). The output of the proportional counters will be subjected to pulse-height analysis by an on-board step-scanning single-channel analyzer with adjustable counting periods. The data will be returned to Earth, via the Viking Orbiter relay system, and the spectra constructed, calibrated, and interpreted here. The instrument is inside the Lander body, and samples are to be delivered to it by the Viking Lander Surface Sampler. Calibration standards are an integral part of the instrument. The results of the investigation will characterize the surface materials of Mars as to elemental composition with accuracies ranging from a few tens of parts per million (at the trace-element level) to a few percent (for major elements) depending on the element in question. Elements of atomic number 11 or less are determined only as a group, though useful estimates of their individual abundances maybe achieved by indirect means. The expected radiation environment will not seriously hamper the measurements. Based on the results, inferences can be drawn regarding (1) the surface mineralogy and lithology; (2) the nature of weathering processes, past and present, and the question of equilibrium between the atmosphere and the surface; and (3) the extent and type of differentiation that the planet has undergone. The Inorganic Chemical Investigation supports and is supported by most other Viking Science investigations.

Icarus↗
USGS1971

On the origin of lunar soil 12033

The lunar soil 12033 is compositionally distinctly different from both the local rocks at the Apollo 12 site and other lunar samples. It must be a recent deposit, else it would not have retained its identity. It contains a meteoritic component which is about 0.59 times as large as that in the more typical Apollo 12 soils. The amount of meteoritic component may be either a fortuitous residuum from the object which produced the 12033 material as crater ejecta, or 12033 may consist of a mixture of an exotic component with the local soil in approximately 41:59 proportions. The available evidence favors the latter interpretation.

Earth and Planetary Science Letters↗
USGS1970

Semimicro chemical and x-ray fluorescence analysis of lunar samples

Major and selected minor elements were determined in seven whole rock fragments, five portions of pulverized lunar rock, and the lunar soil. Three different rock types were represented: vesicular, fine-grained basaltic rocks; medium- to coarse-grained, vuggy gabbroic rocks; and breccia. The ranges (in percent) for the major constituents of the lunar samples are: SiO 2 , 38 to 42; Al 2 O 3 , 8 to 14; total iron as FeO, 15 to 20; MgO, 6 to 8; CaO, 10 to 12; Na 2 O, 0.5 to 1; K 2 O, 0.05 to 0.4; TiO 2 , 8 to 13; MnO, 0.2 to 0.3; and Cr 2 O 3 , 0.2 to 0.4. The high reducing capacity of the samples strongly suggests the presence of Ti(III).

Science↗
USGS1969

The determination of nanogram amounts of Chromium in urine by x-ray fluorescence spectroscopy

Nanogram amounts of chromium can be extracted as oxinate into chloform. By treatment of the chloroform layer 3 M hydrochloric acid, oxinates of other elements and excess of reagent are removed, leaving a chloroform solution of the chromium chelate only. This solution is concentrated and transferred to the top of a small brass rod acting as sample holder. The intensity of the X-ray fluorescence of the Cr Kα line is measured with curved crystal optics. Chromium amounts greater than 5 ng can be detected. The application of the procedure to the analysis of the chromium content of urine is demonstrated.

Analytica Chimica Acta↗
USGS1957

Minor elements in Keweenawan lavas, Michigan

The distribution of minor elements in three basaltic flows of the Keweenawan series, of Michigan, is related to differentiation in the flows. Thus, nickel is most abundant in the early differentiates; nickel, chromium, and barium are generally deficient in the pegmatites, which formed late; whereas copper, vanadium, yttrium, and other minor elements are concentrated in the pegmatites. The minor-element content of individual minerals in the Greenstone flow varies markedly from one mineral to another and seems to depend primarily on the presence or absence in the minerals of major elements for which the minor elements can substitute. Minor elements have substituted most readily for those major elements with similar ionic radii. Valence and electronegativity also seem to influence the ease of substitution. The distribution of other minor elements in copper-bearing lodes of the Michigan copper district shows no apparent relation to copper mineralization.

Michigan↗
USGS1957

Systematic variation of rare-earth elements in cerium-earth minerals

In a continuation of a study reported previously, rare-earth elements and thorium have been determined in monazite, allanite, cerite, bastnaesite, and a number of miscellaneous cerium-earth minerals. A quantity called sigma (∑), which is the sum of the atomic percentages of La, Ce, and Pr, is proposed as an index of composition of all cerium-earth minerals with respect to the rare-earth elements. The value of ∑ for all of the minerals analysed falls between 58 and 92 atomic per cent. Monazites, allanites, and cerites cover the entire observed range, whereas bastnaesites are sharply restricted to the range between 80 and 92 atomic per cent. The minimum value of ∑ for a cerium-earth mineral corresponds to the smallest possible unit-cell size of the mineral. In monazite, this structurally controlled minimum value of ∑ is estimated to be around 30 atomic per cent. Neodymium, because of its abundance, and yttrium, because of its small size, have dominant roles in contraction of the structure. In the other direction, the limit of variation in composition will be reached when lanthanum becomes the sole rare-earth element in a cerium-earth mineral. Cerium-earth minerals from alkalic rocks are all characterized by values of ∑ greater than 80 atomic per cent, indicating that the processes that formed these rocks were unusually efficient in fractionating the rare-earth elements—efficient in the sense that a highly selected assemblage is produced without eliminating the bulk of these elements. Analyses of inner and outer parts of two large crystals of monazite from different deposits show no difference in ∑ in one crystal and a slightly smaller value of ∑ in the outer part of the other crystal compared to the inner part. The ∑ of monazites from pegmatites that intrude genetically related granitic rocks in North Carolina is found to be either higher or lower than the ∑ of monazites in the intruded host rock. These results indicate that the fractionation of the rare-earth elements is not a simple unidirectional process. When a cerium-earth mineral undergoes replacement, its rare-earth elements may be fractionated into two parts, one forming a new mineral with ∑ that is smaller, and the other a second new mineral with ∑ that is larger than that of the original mineral. The complete analysis of a cerium-earth mineral to determine its ∑ is time consuming. The discovery of a direct relationship between ∑ and the Ce/(Nd + Y) atomic ratio in cerium earth minerals allows a rapid determination of ∑ from spectrograms obtained in a previously described method for determining thorium in these minerals.

Geochimica et Cosmochimica Acta↗
USGS1954

A chemical-spectrochemical method for the determination of rare earth elements and thorium in cerium minerals

In a combined chemical-spectrochemical procedure for quantitatively determining rare earth elements in cerium minerals, cerium is determined volumetrically, a total rare earths plus thoria precipitate is separated chemically, the ceria content of the precipitate is raised to 80·0 percent by adding pure ceria, and the resulting mixture is analyzed for lanthanum, praseodymium, neodymium, samarium, gadolinium, yttrium, and thorium spectrochemically by means of the d.c. carbon arc. Spectral lines of singly ionized cerium are used as internal standard lines in the spectrochemical determination which is patterned after Fassel's procedure [1]. Results of testing the method with synthetic mixtures of rare earths and with samples of chemically analyzed cerium minerals show that the coefficient of variation for a quadruplicate determination of any element does not exceed 5·0 (excepting yttrium at concentrations less than 1 percent) and that the method is free of serious systematic error.

Spectrochimica Acta↗
USGS1953

Systematic variation of rare earths in monazite

Ten monazites from widely scattered localities have been analyzed for La, Ce, Pr, Nd, Sm, Gd, Y and Th by means of a combined chemical and emission spectrographic method. The analytical results, calculated to atomic percent of total rare earths (thorium excluded), show a considerable variation in the proportions of every element except praseodymium, which is relatively constant. The general variation trends of the elements may be calculated by assuming that the monazites represent different stages in a fractional precipitation process, and by assuming that there is a gradational increase in the precipitability of rare earth elements with decreasing ionic radius. Fractional precipitation brings about an increase in lanthanum and cerium, little change in praseodymium, and a decrease in neodymium, samarium, gadolinium, and yttrium. Deviations from the calculated lines of variation consist of a simultaneous, abnormal increase or decrease in the proportions of cerium, praseodymium, and neodymium with antipathetic decrease or increase in the proportions of the other elements. These deviations are ascribed to abnormally high or low temperatures that affect the precipitability of the central trio of elements (Ce, Pr, Nd) relatively more than that of the other elements. The following semiquantitative rules have been found useful in describing the composition of rare earths from monazite: 1. The sum of lanthanum and neodymium is very nearly a constant at 42 ± 2 atomic percent. 2. Praseodymium is very nearly constant at 5 ± 1 atomic percent. 3. The sum of Ce, Sm, Gd, and Y is very nearly a constant at 53 ± 3 atomic percent. No correlation could be established between the content of Th and that of any of the rare earth elements.

Geochimica et Cosmochimica Acta↗