Iron speciation related to color of Jurassic sedimentary rocks in Turpan Basin, northwest China

Mesozoic-Cenozoic reddish and green beds are widely distributed in northwest China. Mössbauer spectroscopy revealed that the composition of iron species varies with color in the middle-upper Jurassic sedimentary rocks from the Turpan Basin. Three main kinds of iron species were identified: (1) ferric iron of hematite (hem-Fe³⁺), (2) paramagnetic ferric iron (para-Fe³⁺), and (3) paramagnetic ferrous iron (para-Fe²⁺). Pyrite iron (pyr-Fe²⁺) was revealed only in a few samples. In general, there is a direct correlation between rock color, iron species and total iron content, however, in detail, this relationship is more complicated. The reddish rocks contain higher contents of total iron and hem-Fe³⁺, whereas the gray rocks contain much more para-Fe²⁺. However, relatively low hematite content cannot give red color to rocks, probably due to suppression by other pigments such as organic matter in black or chlorite in green. The dark or green rocks normally contain either only paramagnetic Fe²⁺ and paramagnetic Fe³⁺ species or these two species associated with hematite Fe³⁺, but the relative content of hematite species is lower. The variations of different iron species control lithological properties such as color and also may reflect the sedimentary conditions. Moreover, iron speciation in these rocks is one of the main factors, which result the color features of rocks in remote sensing imagery.This revised version was published online in November 2005 with corrections to the Cover Date.     

Neutron activation analysis of Japanese standard rocks

Neutron activation analyses were performed for the newly issued reference rocks, GSJ JA-1 and JB-2, and also for the widely distributed GSJ JG-1 and JB-1. The contents of fourteen elements could be newly determined for the former two rocks and those of eleven elements were re-determined for the latter rocks.     

Neutron activation analysis of rare earth elements in alered volcanic rocks /palagonite/ from a seamount

By means of INAA, REEs in the dredged rocks from a seamount /KH73-4-2/ in the East Mariana Basin were determined. Based on the REE patterns, the rocks are classified into two groups despite of alteration: highly altered palagonite of oceanic-island tholeiitic nature, and relatively fresh basaltic-andesitic rocks of alkaline rock nature.     

Accurate and efficient determination of boron content in volcanic rocks by neutron induced prompt gamma-ray analysis

An accurate and efficient analytical method using neutron-induced prompt γ-ray was developed for the determination of boron contents in volcanic rocks. We corrected the effect of sample geometry and flux fluctuation by using silicon as an internal standard. However, we found that the slopes of the calibration line vary among volcanic samples with different matrix. Because the increase of boron activity correlates positively with γ-ray count rate of hydrogen (water), we call this as the hydrogen effect. The hydrogen effect was confirmed by our experiment in which the boron activities showed systematic increase with the amount of added hydrogen (water). Most volcanic rocks, however, contain little water (<2 wt.%) to show this effect. We determined boron contents in various volcanic rocks in order to confirm the validity of the procedure that we established. The analyzed boron contents agreed well with the previous reported values. For efficient PGA of boron in volcanic rocks, we recommend JB-2 (GSJ standard rock) as a single geochemical standard, because of its high boron content (31.2 ppm).     

Joint determination of fluorine and chlorine in granitic rocks with ion-selective electrodes

This enables both fluorine and chlorine in granitic rocks to be determined with a single sample. A rapid technique, using fusions in culture tubes, and a slower technique, employing fusions in platinum crucibles are described. The culture-tube technique is suitable for geochemical exploration and employs an oxidizing flux so that sulphide-bearing rocks can be analysed. The platinum-crucible technique yields fluorine and chlorine results for the standard rocks G-2 and GSP-1 that are comparable in value and precision to those obtained by other analytical methods. It is faster, easier to manipulate and yields higher fluorine values than the existing joint spectrophotometric method.     

Determination of total iron in standard rocks by spectrophotometric titration with EDTA

A method for the determination of total iron in silicate rocks is described. It is based on spectrophotometric titration of iron(III) with EDTA after decomposition in a PTFE bomb. No prior separation of interfering elements is needed. The method was tested by analysis of the U.S. Geological Survey reference rocks G-2, AGV-1, GSP-1, BCR-1 and PCC-1. The same sample solutions were also analysed by atomic-absorption spectrophotometry. The agreement with published and recommended values was good.     

Precision analyses of manganese in rocks by neutron activation analysis

A simple and rapid procedure for the determination of manganese in rocks by neutron activation and γ-spectrometry is presented. The precision of the method calculated from analyses of standard rocks is of the order 1.5–2%, and an accuracy of ±2% is attainable. The method is applicable to most types of geological samples, and should be superior to conventional methods used in rock analysis.     

Neutron activation determination of noble metals in rocks: A rapid radiochemical separation based on tellurium coprecipitation

A procedure is described for the determination of Pd, Au, Ir, and Pt in rocks at the ppb concentration level. After irradiation with thermal neutrons, powdered rock samples are fused with carriers and Na₂O₂−NaOH. The fusion cake is dissolved in dilute HCl, and the activated noble metals and carriers are coprecipitated as a group with Te, using Sn²⁺ as a reductant. Gamma and X-rays are counted on semi-conductor Ge deterctors. Yields are determined by reirradiation. Results are given for several rocks, including U.S.G.S. standards PCC-1 and W-1.     

Determination of gallium in geological materials by graphite-furnace atomic-absorption spectrometry

A graphite-furnace atomic-absorption spectrometric method has been worked out for the determination of traces of gallium in silicate rocks and minerals. The samples are opened up by fusion with a lithium carbonate-boric acid mixture and the cake is taken up with 2M nitric acid. Addition of nickel nitrate to this solution elminates the severe matrix effects allowing gallium solutions in nitric acid to be used as calibration standards. No separations are necessary. Results are quoted for 14 standard silicate rocks and two minerals. The RSD is 2.9%, and the sensitivity is 27 pg of gallium for 1% absorption.     

Simple radiochemical neutron-activation method for the determination of uranium in ultramafic rocks

A radiochemical neutron-activation method for the determination of trace concentrations of uranium in rocks is described. The method is based on separation of 23·5-min ²³⁹U after alkaline fusion by extraction with tri-n-butyl phosphate from moderately concentrated nitric acid, followed by measurement of the 74-keV γ-ray with a Ge(Li) detector. The limit of detection is 0·2 ng of U under the present conditions, and the precision at the 0·005 ppm level is about 10%. The method is especially useful for determination of uranium in ultramafic rocks.     

Hydrothermal extraction of potassium,sodium, rubidium and cesium from rocks by lithium hydroxide and determination at very low natural levels

The selective extraction of Na, K, Rb and Cs from rocks is described. The method is particularly designed for low levels of rubidium and cesium in basic and ultrabasic rocks. The rocks are decomposed with lithium hydroxide solution at 180°C. Only part of the aluminium and chromium accompany the alkali metals into solution; all other rock constitutents are left behind as insoluble lithium silicate, hydroxides of divalent metals, etc. Concentration of rubidium and cesium too low to be determined directly by flame emission spectrometry are pre-concentrated up to 25-fold by liquid-liquid extraction. Quantitative recovery (>99.5%) of the two metals is achieved by coprecipitation with potassium tetraphenylboron within the organic phase (di-isobutyl ketone) for subsequent back-extraction and dissolution in an acidic aqueous phase. Detection limits are 1 mg kg^?1 Na or K, 0.1 mg kg^?1 Rb and 0.05 mg kg^?1 Cs in the rock for the direct determination and 0.003 mg kg^?1 Rb and 0.001 mg kg^?1 Cs after preconcentration. Methods are described for the purification of lithium hydroxide and the potassium nitrate used as carrier. Results are presented for the Na₂ O, K₂O, Rb and Cs contents and the K/Rb values for 23 geochemical references samples (basic and ultrabasic rocks, and iron formation samples).     

Source Rocks of the Caledonian-Age Granitoid Rocks in Wanyanshan-Zhuguangshan, Southeast China (Ⅱ)——Topological Analysis in Isotopic Multispace

Topological analysis in Sr-Nd-O-Pb_3 six-dimensional isotopic space suggests that the source rocks of the Caledonian-age granitoid rocks in Wanyangshan-Zhuguangshan, southeast China, comprise three end-member components. Isotopic mixing model discrimination indicates that the granitoid rocks were produced through mixing of the three componentsin varying proportions. Comprehensive study of multiple isotopic systems and geochemistry of the granitoid rocks suggests that the three end-member components were crustal rocks which are continent-derived sediments, geosycline sediments and altered basic volcanic rocks.     

Determination of trace iodine in rock samples by epiterhmal neutron activation analysis involving rapid radiochemical separation

Applying rapid radiochemical separation of iodine coupled with epithermal neutron activation, we reliably determined trace amounts /6–95 ng/ of iodine in rock samples such as sedimentary rocks and chondritic meteorites. Our data on meteorites are in good agreement with literature values, but for sedimentary rocks the present data were systematically lower than the literature values. Based on the data from duplicate analyses of some sedimentary rocks and the results of tracer experiments employed parallel to the rock analyses, we concluded that the analytical results obtained in this work for sedimentary rocks were more reliable than the literature values.     

Pseudocyclic activation analysis of geological material

A pseudocyclic activation system has been installed at the Ecole Polytechnique SLOWPOKE reactor. It is shown that, for analyses of geological material with short-lived nuclides, pseudocyclic activation is preferable to cyclic activation because it avoids the buildup of²⁸Al activity. The total experiment time is reasonable when several sample are analyzed. The possibilities of the technique were illustrated with the analysis of nine well-known silicate rocks. With n cycles an improvement in precision approaching n^1/2 was achieved. The detection limits in silicate rocks were determined for 18 elements using thermal and epithermal irradiation and 25 cycles.     

Radiochemical neutron activation analysis of trace lanthanoids in geological and cosmochemical samples

In order to determine trace lanthanoids in geological and cosmochemical samples, an analytical procedure for radiochemical neutron activation analysis (RNAA) was developed, where lanthanoids are radio-chemically purified through precipitations of hydroxides and fluorides, and cation exchange using HBr as an eluent. Chemical yields are determined by reactivation. The procedure was applied to the Allende meteorite and geological standard rocks. Our data for Allende are in excellent agreement with literature values, and those values for standard rocks, JP-1 (peridotite) and JF-2 (feldspar), in which lanthanoids are depleted by orders of 1 to 2 compared with those in Allende, seem to be reasonable, although not properly evaluated because of large scatterings in their literature data. This suggests that the present RNAA procedure is highly effective in determining trace lanthanoids (less than 1 ng) in rock samples.     

The analysis of inorganic siliceous materials by atomic absorption spectrophotometry and the hydrofluoric acid decomposition technique : Part I. the analysis of silicate rocks

The analysis of various inorganic siliceous materials of geological and industrial interest is discussed. The methods proposed are based on decomposition of a single sample by hydrofluoric acid and determination by atomic absorption spectrophotometry of up to 10 constituents. General procedures are described, and details are given for the determination of silicon, aluminium, total iron, magnesium, calcium, sodium, potassium, titanium and manganese in silicate rocks. Analytical data are given for the analysis of reference rocks G-2 and W-1.     

Analysis for the rare-earth elements by neutron activation and Ge(Li) spectrometry

A procedure for analysis of 12 of the rare-earths, tested on more than a hundred samples of rocks and minerals, is described. Carrier is added for each element to be determined. Samples are fused with Na₂O₂. The rare-earths are separated as a group, then precipitated and mounted as oxalates for Ge(Li) spectrometry. Following radioassay, chemical yields for the individual rare-earths are obtained by irradiation and counting of the carrier. About two months are needed to obtain complete data for a set of four samples, but many samples are analyzed concurrently. The precision and accuracy exceed ±5 per cent for 10 of the elements in 0.1 to 0.5 g samples of common rocks.     

Distribution and Composition of Organic Matter in Oil- and Bitumen-cotaining Rocks in Deposits of Different Ages

The core samples of oil- and bitumen-containing rocks from Tatarstan's deposits of different ages were studied by thermal analysis methods (DTA, TG, DTG). Based on the obtained data, a procedure was elaborated for determining the enclosed organic matter content and the index of its fraction composition. A significant increase of the organic matter content in the core and its enrichment in high-molecular aromatic structures were shown to occur for the oil-containing rock samples when passing from the Devonian to Carboniferous and Permian deposits. The core samples of the Devonian oil-containing rocks may be divided into three groups: the samples taken from the zones where waste water flooding has been started relatively recently (1), or fresh water flooding has been carried on for a long time (2) and the samples of rock containing clay minerals as impurities. Thus, thermal analysis can be used in geochemical studies to identify the organic matter enclosed by oil- and bitumen-containing rocks. This revised version was published online in August 2006 with corrections to the Cover Date.     

Determination of uranium in rocks by instrumental activation-analysis using epithermal neutrons

A rapid non-destructive neutron-activation method for the determination of uranium in rocks is described. The method is based on activation with epithermal neutrons and subsequent measurement of the 74 keV gamma-ray of (239)U. Results given for some standard rocks are in good agreement with literature data. The precision of the method is about 5 % and the limit of detection is of the order of 0.1 ppm in silicate rocks.     

Determination of yttrium and rare-earth elements in rocks by graphite-furnace atomic-absorption spectrometry

With use of synthetic solutions and several international standard reference materials a method has been developed for determining traces of Y, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in rocks by electrothermal atomization in a pyrolytically-coated graphite furnace. Depending on the element, the sensitivity is of the order of 10(-9)-10(-12) g at 2500 degrees . To avoid matrix interferences the lanthanides are separated from the common elements by co-precipitation with calcium and iron as carriers. The data for Canadian reference rock SY-2 (syenite), U.S.G.S. reference rocks W-2 (diabase), DNC-1 (diabase) and BIR-1 (basalt), and South African reference rock NIM-18/69 (carbonatite) obtained by graphite-furnace atomization are compared with the values obtained by flame atomic-absorption. The results are in good agreement with literature values.