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J.J. Rowe

Publications and source records attributed to J.J. Rowe.

15 recordsLinked to original sources

Molybdenum blue reaction and determination of phosphorus in waters containing arsenic, silicon, and germanium

Microgram amounts of phosphate are usually determined by the molybdenum blue reaction, but this reaction is not specific for phosphorus. The research established the range of conditions under which phosphate, arsenate, silicate, and germanate give the molybdenum blue reaction for differentiating these elements, and developed a method for the determination of phosphate in waters containing up to 10 p.p.m. of the oxides of germanium, arsenic(V), and silicon. With stannous chloride or 1-amino-2-naphthol-4-sulfonic acid as the reducing agent no conditions were found for distinguishing silicate from germanate and phosphate from arsenate. In the recommended procedure the phosphate is concentrated by coprecipitation on aluminum hydroxide, and coprecipitated arsenic, germanium, and silicon are volatilized by a mixture of hydrofluoric, hydrochloric, and hydrobromic acids prior to the determination of phosphate. The authors are able to report that the total phosphorus content of several samples of sea water from the Gulf of Mexico ranged from 0.018 to 0.059 mg. of phosphorus pentoxide per liter of water.

Analytical Chemistry

Chemical analysis of 617 coal samples from the Eastern United States

This report includes all the analytical data on 617 coal samples from 8 states east of the Mississippi River. The samples from each state are, Pennsylvania 71, Ohio 40, West Virginia 252, Virginia 72, Kentucky 27, Tennessee 27, Alabama 20, and Indiana 108. The U.S. Geological Survey has quantitatively determined the amounts of 35 major, minor and trace elements in each sample. It has also searched for 35 other trace elements using semi-quantitative spectrographic methods. In addition, the Coal Analysis Section of the Department of Energy has provided proximate and ultimate analyses, Btu, forms of sulfur, free swelling index, and ash fusion temperatures on 491 samples. Comparison of the geometric means of these samples with 331 bituminous coal samples of the Appalachian region reported by Swanson and others (1976) are as follows. As shown by the means for ultimate and proximate analyses small differences exist between the two sets of data, only the moisture content and oxygen are significantly different. The forms of sulfur and heat of combustion are also similar. The means for the major and minor oxides in ash are similar for SiO 2 , Al 2 O 3 , CaO, MgO, K 2 O 3 and TiO 2 . Na 2 O is significantly lower and Fe 2 O 3 and MnO higher in the analyses of the 617 samples of this report. Most means for the trace elements in the coals studied for this report are lower. Only Be is significantly higher in these coals.

Alabama, Indiana, Kentucky, Ohio, Pennsylvania, Te

Application of epithermal neutron activation in multielement analysis of silicate rocks employing both coaxial Ge(Li) and low energy photon detector systems

The instrumental activation analysis of silicate rocks using epithermal neutrons has been studied using both high resolution coaxial Ge(Li) detectors and low energy photon detectors, and applied to the determination of 23 elements in eight new U.S.G.S. standard rocks. The analytical use X-ray peaks associated with electron capture or internal conversion processes has been evaluated. Of 28 elements which can be considered to be determinable by instrumental means, the epithermal activation approach is capable of giving improved sensitivity and precision in 16 cases, over the normal INAA procedure. In eleven cases the use of the low energy photon detector is thought to show advantages over convertional coaxial Ge(Li) spectroscopy. ?? 1977 Akade??miai Kiado??.

Journal of Radioanalytical Chemistry

Determination of 30 elements in coal and fly ash by thermal and epithermal neutron-activation analysis

Thirty elements are determined in coal and fly ash by instrumental neutron-activation analysis using both thermal and epithermal irradiation. Gamma-ray spectra were recorded 7 and 20 days after the irradiations. The procedure is applicable to the routine analysis of coals and fly ash. Epithermal irradiation was found preferable for the determination of Ni, Zn, As, Se, Br, Rb, Sr, Mo, Sb, Cs, Ba, Sm, Tb, Hf, Ta, W, Th and U, whereas thermal irradiation was best for Sc, Cr, Fe, Co, La, Ce, Nd, Eu, Yb and Lu. Results for SRM 1632 (coal) and SRM 1633 (fly ash) agree with those of other investigators.

Talanta

Determination of 22 minor and trace elements in 8 new USGS standard rocks by instrumental activation analysis with epithermal neutrons

Epithermal neutron-activation analyses results of the 8 new USGS standard rocks are compared with results by spectrographic, X-ray fluorimetric, atomic absorption, radiochemical neutron-activation, instrumental neutron-activation (thermal neutrons), isotope-dilution mass spectrometric, spectrofluorimetric, radioisotopic dilution and delayed-neutron techniques for 22 elements. Results indicate the technique to be useful and dependable especially for Ni, Se, Rb, Sr, Mo, Ba, Tm, Ta, Th and U.

Journal of Research of the U.S. Geological Survey

Fractionation of gold in a differentiated tholeiitic dolerite

Gold content was determined, by neutron-activation analysis, in samples from a drill core through the Great Lake sheet, Tasmania, a differentiated tholeiitic dolerite. The gold content of parts of the core seems to be related to the mafic index. The variation of gold content with depth and mafic index is similar to that of copper, indicating that gold and copper may have been concomitantly crystallized from the magma.

Chemical Geology

The ternary system K2SO4 MgSO4 CaSO4

Melting and subsolidus relations in the system K 2 SO 4 MgSO 4 CaSO 4 were studied using heating-cooling curves, differential thermal analysis, optics, X-ray diffraction at room and high temperatures and by quenching techniques. Previous investigators were unable to study the binary MgSO 4 CaSO 4 system and the adjacent area in the ternary system because of the decomposition of MgSO 4 and CaSO 4 at high temperatures. This problem was partly overcome by a novel sealed-tube quenching method, by hydrothermal synthesis, and by long-time heating in the solidus. As a result of this study, we found: (1) a new compound, CaSO 4 ·3MgSO 4 (m.p. 1201°C) with a field extending into the ternary system; (2) a high temperature form of MgSO 4 with a sluggishly reversible inversion. An X-ray diffraction pattern for this polymorphic form is given; (3) the inversion of β-CaSO 4 (anhydrite) to α-CaSO 4 at 1195°C, in agreement with grahmann ; (1) (4) the melting point of MgSO 4 is 1136°C and that of CaSO 4 is 1462°C (using sealed tube methods to prevent decomposition of the sulphates); (5) calcium langbeinite (K 2 SO 4 ·2CaSO 4 ) is the only compound in the K 2 SO 4 CaSO 4 binary system. This resolved discrepancies in the results of previous investigators; (6) a continuous solid solution series between congruently melting K 2 SOP 4 ·2MgSO 4 (langbeinite) and incongruently melting K 2 SO 4 ·2CaSO 4 (calcium langbeinite); (7) the liquidus in the ternary system consists of primary phase fields of K 2 SO 4 , MgSO 4 , CaSO 4 , langbeinite-calcium langbeinite solid solution, and CaSO 4 ·3MgSO 4 . The CaSO 4 field extends over a large portion of the system. Previously reported fields for the compounds (K 2 SO 4 ·MgSO 4 ·nCaSO 4 ), K 2 SO 4 ·3CaSO 4 and K 2 SO 4 ·CaSO 4 were not found; (8) a minimum in the ternary system at: 740°C, 25% MgSO 4 , 6% CaSO 4 , 69% K 2 SO 4 ; and ternary eutectics at 882°C, 49% MgSO 4 , 19% CaSO 4 , 32% K 2 SO 4 ; and 880°, 67·5% MgSO 4 , 5% CaSO 4 , 27·5% K 2 SO 4 .

Journal of Inorganic and Nuclear Chemistry

The binary system K2SO4CaSO4

The binary system K 2 SO 4 CaSO 4 was studied by means of heating-cooling curves, differential thermal analysis, high-temperature quenching technique and by means of a heating stage mounted on an X-ray diffractometer. Compositions and quench products were identified optically and by X-ray. Limited solid solution of CaSO 4 in K 2 SO 4 was found. There is a eutectic at 875°C and 34 wt. per cent CaSO 4 . Calcium langbeinite melts incongruently at 1011°C. The melting-point of CaSO 4 (1462°C) was determined by the quenching technique using sealed platinum tubes. The only intermediate crystalline phase found in the system is K 2 SO 4 ·2CaSO 4 (calcium langbeinite).

Journal of Inorganic and Nuclear Chemistry

Solution of rocks and refractory minerals by acids at high temperatures and pressures. Determination of silica after decomposition with hydrofluoric acid

A modified Morey bomb was designed which contains a removable nichromecased 3.5-ml platinium crucible. This bomb is particularly useful for decompositions of refractory samples for micro- and semimicro-analysis. Temperatures of 400–450° and pressures estimated as great as 6000 p.s.i. were maintained in the bomb for periods as long as 24 h. Complete decompositions of rocks, garnet, beryl, chrysoberyl, phenacite, sapphirine, and kyanite were obtained with hydrofluoric acid or a mixture of hydrofluoric and sulfuric acids; the decomposition of chrome refractory was made with hydrochloric acid. Aluminum-rich samples formed difficultly soluble aluminum fluoride precipitates. Because no volatilization losses occur, silica can be determined on sample solutions by a molybdenum-blue procedure using aluminum(III) to complex interfering fluoride.

Analytica Chimica Acta

The system K2Mg2(SO4)3 (langbeinite)-K2Ca2(SO4)3 (calcium-langbeinite)

The join between the compositions K 2 Mg 2 (SO 4 ) 3 and K 2 Ca 2 (SO 4 ) 3 was studied by means of high-temperature equilibrium quenching techniques and by means of a heating stage mounted on an X-ray diffractometer. Complete solid solution exists in the system, but at 25°C members of the solid solution series are isometric only in the composition range 0–73·5 wt. per cent K 2 Ca 2 (SO 4 ) 3 . At compositions richer in K 2 Ca 2 (SO 4 ) 3 than 73·5 wt. per cent, members of the series are optically biaxial. At higher temperatures members of the solid solution series are isometric at successively more calcium-rich compositions and pure K 2 Ca 2 (SO 4 ) 3 is isometric above about 200 ± 2°C. The system is not binary, as mixtures richer in K 2 Ca 2 (SO 4 ) 3 than 42 wt. per cent decompose with the formation of liquid and CaSO 4 .

Journal of Inorganic and Nuclear Chemistry

Releasing-addition method for the flame-photometric determination of calcium in thermal waters

Study of the interferences of silica and sulfate in the flame-photometric determination of calcium in thermal waters has led to the development of a method requiring no prior chemical separations. The interference effects of silica, sulfate, potassium, sodium, aluminum, and phosphate are overcome by an addition technique coupled with the use of magnesium as a releasing agent.

Geochimica et Cosmochimica Acta

The solubility of quartz in water in the temperature interval from 25° to 300° C

The solubility of quartz in water was investigated by three sets of experiments at 1000 atm P H 2 O and temperatures ranging from 45° to 300°C at water pressures appropriate for the coexistence of three phases, gaseous water, liquid, and quartz, at temperatures ranging from 69° to 240°C a long term study of the dissolution of quartz grains which were continuously tumbled in water at room temperature. Saturated silica solutions in equilibrium with quartz were obtained in a few days at temperatures above 100°C. Equilibrium is shown by reproducible results for runs of different durations and by the precipitation of quartz from initially supersaturated solutions. The differential heat of solution derived from the data obtained at 1000 atm pressure is 5.38 kcal/mole. At room temperature and pressure, highly supersaturated silica solutions were obtained by continuously rotating quartz grains and water in plastic bottles at 75 rev/min. In one run the amount of silica in solution increased to a maximum value of 395 p.p.m. after 370 days. Another run reached 80 p.p.m. silica after 386 days and then dropped to 6 p.p.m. silica. It is concluded that quartz was precipitated at room temperature from this supersaturated solution and that 6 p.p.m. is essentially the true solubility of quartz at 25°C. In contrast to the runs rotated at 75 rev/min, quartz grains, and also silica glass grains, continuously rotated in water at rev/min, each contributed less than 1 p.p.m. colorimetric silica into solution after 1 year. Thus, vigorous agitation of the liquid is necessary to remove dissolved silica from the vicinity of surfaces of both quartz and glass. Two significant factors that may have contributed to the formation of supersaturated silica solutions in the runs rotated at 75 rev/min at room temperature are stresses and structural irregularities at the surfaces of the crushed quartz grains, which contributed silica into solution more readily than well crystallized quartz the very slow rate at which dissolved silica polymerizes to species appropriate to act as nuclei for quartz growth. At the termination of the runs rotated at 75 rev/min, spikelike projections were present on many of the quartz grains. These are interpreted as indicating that abrasion was not the dominant cause for the great supersaturations which were obtained.

Geochimica et Cosmochimica Acta