Comparison of Two Sample Preparation Methods for X‐Ray Fluorescence Spectrometry in the Determination of Ni and Cr

Pressed powder pellets and fused beads or glass disks are routinely used in X‐ray fluorescence spectrometry for the determination of major and trace elements, respectively, in geological materials. In order to evaluate the performance of these two sample preparation methods, we determined Ni and Cr concentrations of fourteen RMs from Japan, France and South Africa, and eighty‐five igneous and three sedimentary rock samples from Mexico in both powder pellets and glass beads. We also computed new values of statistical parameters for RMs from an outlier‐based multiple‐test method and compared them with the literature mean and confidence limit values. The results showed that the multiple‐test method provided more reliable central tendency and dispersion parameters for RMs than those obtained previously from the two or three standard deviation method, or from robust methods. The powder pellet and fused bead sample preparation methods provided consistent results for Ni and Cr at concentration levels > 50 μg g^?1 in this application; for lower concentration levels, however, these methods showed somewhat greater differences. For quantitative comparisons, both ordinary and weighted least‐squares linear regression models were used to show that the two sample preparation methods provided generally unbiased results.     

Multi‐Element Determination of Trace Elements in Natural Water Reference Materials by ICP‐SFMS after Tm Addition and Iron Co‐precipitation

We report on an improved method for determining trace element abundances in seawater and other natural waters. The analytical procedure involves co‐precipitation on iron hydroxides after addition of a Tm spike, and measurement by inductively coupled plasma‐sector field mass spectrometry (ICP‐SFMS). The validity of the method was assessed through a series of co‐precipitation experiments, using ultra‐diluted solutions of a certified rock reference material (BIR‐1). Results obtained for four natural water reference materials (NASS‐5, CASS‐4, SLEW‐3, SLRS‐4) are in agreement with published working values for rare earth elements, yttrium, vanadium and, when available, for hafnium, zirconium, thorium and scandium. A set of proposed values with uncertainties typically better than 8% RSD is proposed for Hf, Zr and Th.     

Precise Determination of Silicon Isotopes in Silicate Rock Reference Materials by MC‐ICP‐MS

A HF‐free sample preparation method was used to purify silicon in twelve geological RMs. Silicon isotope compositions were determined using a Neptune instrument multi‐collector‐ICP‐MS in high‐resolution mode, which allowed separation of the silicon isotope plateaus from their interferences. A 1 μg g^‐1 Mg spike was added to each sample and standard solution for online mass bias drift correction. δ³⁰Si and δ²⁹Si values are expressed in per mil (‰), relative to the NIST SRM 8546 (NBS‐28) international isotopic RM. The total variation of δ³⁰Si in the geological reference samples analysed in this study ranged from ‐0.13‰ to ‐0.29‰. Comparison with δ²⁹Si values shows that these isotopic fractionations were mass dependent. IRMM‐17 yielded a δ³⁰Si value of ‐1.41 ± 0.07‰ (2s, n = 12) in agreement with previous data. The long‐term reproducibility for natural samples obtained on BHVO‐2 yielded δ³⁰Si = ‐0.27 ± 0.08‰ (2s, n = 42) on a 12 month time scale. An in‐house Si reference sample was produced to check for the long‐term reproducibility of a mono‐elemental sample solution; this yielded a comparable uncertainty of ± 0.07‰ (2s, n = 24) over 5 months.     

GSD‐1G and MPI‐DING Reference Glasses for In Situ and Bulk Isotopic Determination

This paper contains the results of an extensive isotopic study of United States Geological Survey GSD‐1G and MPI‐DING reference glasses. Thirteen different laboratories were involved using high‐precision bulk (TIMS, MC‐ICP‐MS) and microanalytical (LA‐MC‐ICP‐MS, LA‐ICP‐MS) techniques. Detailed studies were performed to demonstrate the large‐scale and small‐scale homogeneity of the reference glasses. Together with previously published isotopic data from ten other laboratories, preliminary reference and information values as well as their uncertainties at the 95% confidence level were determined for H, O, Li, B, Si, Ca, Sr, Nd, Hf, Pb, Th and U isotopes using the recommendations of the International Association of Geoanalysts for certification of reference materials. Our results indicate that GSD‐1G and the MPI‐DING glasses are suitable reference materials for microanalytical and bulk analytical purposes.     

In situ experimental decomposition studies in estuaries: A comparison of Phragmites australis and Fucus vesiculosus

The decomposition rates of Phragmites australis and Fucus vesiculosus were experimentally determined in an estuarine system using the leaf-bag technique. The study was conducted in fifteen sites arranged in five areas, extending from freshwater, outside the tidal range, to the marine environment, near the mouth of the estuary. The leaf-bags (5 mm mesh), were set up with 3.0 g of dried substrate, submerged in the experimental sites at day 0 and collected at days 3, 7, 15, 30 and 60, to follow biomass loss. The biomass loss through the leaching phase (day 3) was about 16% for Phragmites australis and 33% for Fucus vesiculosus and was independent of salinity for both substrates. The difference in the remaining biomass between the two species increased with time and the decomposition rates differed along the salinity gradient. For F. vesiculosus, the decomposition rate was highest near the mouth of the estuary, corresponding to the preferential distribution area of the algae, and decreased towards freshwater. For Phragmites australis, the fastest decay was observed in the mid estuary, where Phragmites australis occurs naturally, confirming previous studies. The decomposition rates measured at different time intervals (0–15, 0–30 and 0–60 days) were always higher for the algae and decreased with time for both species. These results indicate that the use of decomposition rates as a measure of ecosystem integrity or quality status in transitional waters will not be straightforward and must take into account, among others, the test species, the study area positioning along the estuarine gradient, and the time interval for the calculation of the decomposition rate.     

Pollen‐ and diatom based environmental history since the Last Glacial Maximum from the Andean core Fúquene‐7, Colombia

The late Pleistocene–Holocene ecological and limnological history of Lake Fúquene (2580 m a.s.l.), in the Colombian Andes, is reconstructed on the basis of diatom, pollen and sediment analyses of the upper 7 m of the core Fúquene‐7. Time control is provided by 11 accelerator mass spectrometry (AMS) ¹⁴C dates ranging from 19 670 ± 240 to 6040 ± 60 yr BP. In this paper we present the evolution of the lake and its surroundings. Glacial times were cold and dry, lake‐levels were low and the area was surrounded by paramo and subparamo vegetation. Late‐glacial conditions were warm and humid. The El Abra Stadial, a Younger Dryas equivalent, is reflected by a gap in the sedimentary record, a consequence of the cessation of deposition owing to a drop in lake‐level. The early Holocene was warm and humid; at this time the lake reached its maximum extension and was surrounded by Andean forest. The onset of the drier climate prevailing today took place in the middle Holocene, a process that is reflected earlier in the diatom and sediment records than in the pollen records. In the late Holocene human activity reduced the forest and transformed the landscape. Climate patterns from the Late‐glacial and throughout the Holocene, as represented in our record, are similar to other records from Colombia and northern South America (the Caribbean, Venezuela and Panama) and suggest that the changes in lake‐level were the result of precipitation variations driven by latitudinal shifts of the Intertropical Convergence Zone. Copyright © 2003 John Wiley & Sons, Ltd.     

HUMBOLDT'S NODES AND MODES OF INTERDISCIPLINARY ENVIRONMENTAL SCIENCE IN THE ANDEAN WORLD*

ABSTRACT. Alexander von Humboldt engaged in a staggering array of diverse experiences in the Andes and adjoining lowlands of northwestern South America between 1801 and 1803. Yet examination of Humboldt's diaries, letters, and published works shows how his principal activities in the Andes centered on three interests: mining and geological landscapes; communications and cartography; and use and distribution of the quinine‐yielding cinchona trees. Each node represented a pragmatic concern dealing with environmental resources in the context of the Andes. To pursue these interests in his Andean field studies, Humboldt relied on varied cultural interactions and vast social networks for knowledge exchange, in addition to extensive textual comparisons. These modes of inquiry dovetailed with his pragmatic interests and his open‐ended intellectual curiosity. Fertile combinations in his Andean studies provided the foundation and main testing ground for Humboldt's fused nature‐culture approach as well as his contributions to early geography and interdisciplinary environmental science.     

Small‐scale faulting,topographic steps and seismic ruptures in the Alhambra (Granada,southeast Spain

The Alhambra (14th century AD ) in Granada (southeast Spain) is built at the summit of a Pliocene to Lower Pleistocene conglomeratic formation. Tens of small‐scale normal faults crop out along the northern hillslope of the Alhambra, which have a N130–N150°E strike, dipping 65–75° mostly to the southwest. These are closely spaced faults (approximately 5–30 m) with centimetre to several metre displacements. Several topographic steps in this area coincide with hectometre‐ to kilometre‐scale faults with the same kinematics as the small‐scale ones. Some of these faults appear to be active and related to the present seismicity detected in this region, and associated with the cracks and other damage observed in the Alhambra. Several focal mechanisms calculated in this study are in accordance with the dominant NW–SE orientated normal faults. We interpret that the topographic steps of these faults are a consequence of repeated earthquakes during the past 800 ka. The last large earthquake of approximately 5.1 magnitude in this area occurred in 1431, destroying the Alixares Palace, the Arabian fence and part of the Alhambra wall. We consider the seismic risk associated with these faults to be moderate, as the displacement is partitioned into several hectometre‐ to kilometre‐scale faults. Copyright © 2004 John Wiley & Sons, Ltd.     

Rock Glaciers in the Patagonian Andes: An Inventory for the Monte San Lorenzo (Cerro Cochrane) Massif, 47° S

Although rock glaciers in the Central and Desert Andes of Argentina and Chile have been previously studied in detail, much less attention has been paid to the occurrence of these permafrost forms in Patagonia. Recently, however, the establishment of the Argentinean Glacier Inventory program, which intends to inventory and monitor all ice masses along the Argentinean Andes, has started a large amount of new geocryological research. The project is designed to provide reliable and worldwide comparable results, supported by well established technical procedures and background information. Presented here is the first rock glacier inventory of the Monte San Lorenzo (Cerro Cochrane) region in the southern Patagonian Andes. A total of 130 intact (9.86 km²) and 47 fossil (1.45 km²) landforms were inventoried using two 2.5 m resolution ALOS Panchromatic Remote‐sensing Instruments for Stereo Mapping images. Since the Argentinean federal initiative described above legally protects all rock glaciers in the country as water reserves, and due to the little scientific knowledge concerning rock glaciers in the vast majority of the Patagonian Andes, this inventory provides an important basis for political decision‐making and opens further geocryological research avenues for the Patagonian region in general.