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We report on the design and performance of an improved duoplasmatron ion source for secondary ion mass spectrometers. The source is designed specifically to optimize extraction of negative oxygen ions while suppressing electron extraction using a built-in magnetic asymmetry in the anode electrode. Other changes from conventional designs are (a) drilling the ion extraction aperture directly into the magnetic steel anode rather than in a refractory (nonmagnetic) metal insert, thereby eliminating a magnetic “hole” that acts to counter the desired magnetic concentration of the discharge at the aperture and (b) forming the anode into a conical shape convex toward the intermediate electrode to increase the magnetic field concentration at the extraction aperture, hence the term “Canode.” The built-in magnetic asymmetry allows the width and shape of the intermediate electrode to be varied to further optimize magnetic concentration of the discharge. Tests were performed with both ims 6f and NanoSIMS 50L instruments manufactured by Cameca Instruments, Inc. (Fitchburg, WI, USA). In the ims 6f, the Canode design gave O− primary ion currents up to a factor of five greater than the factory ion source design. In the NanoSIMS 50L, the Canode source produced a focused O− ion beam at the sample with a diameter of 50 nm, identical to the performance of the radio-frequency Hyperion ion source developed by Oregon Physics (Beaverton, OR, USA) and offered as an option by Cameca. 

Clay dehydration at great depth generates fluids and overpressures in organic-rich sediments that can release isotopically light boron from mature organic matter, producing 10B-rich fluids. The B can be incorporated into the tetrahedral sites of authigenic illite during the illitization of smectite. Therefore, the crystal-chemical and geochemical characterization of illite, smectite or interlayered illite–smectite clay minerals can be an indicator of depth (temperature) and reactions with the basin fluids. The aim of this study was to determine the detailed clay mineralogy, B-content and isotopic composition in illite–smectite rich samples of mud volcanoes from the Gulf of Cádiz, in order to evaluate interactions of hydrocarbon-rich fluids with clays. Molecular modeling of the illite structure was performed, using electron density functional theory (DFT) methods to examine the phenomenon of B incorporation into illite at the atomic level. We found that it is energetically preferable for B to reside in the tetrahedral sites replacing Si atoms than in the interlayer of expandable clays. The B abundances in this study are high and consistent with previous results of B data on interstitial fluids, suggesting that hydrocarbon-related fluids approaching temperatures of methane generation (150 °C) are the likely source of B-rich illite in the studied samples. 

Secondary ion mass spectrometry techniques are used to study trace elements in organic samples where matrix compositions vary spatially. This study was conducted to develop calibrations for lithium content and lithium isotope measurements in kerogen. Known concentrations of Li ions (⁶Li and⁷Li) were implanted into organic polymers, with a range of H/C and O/C ratios similar to kerogen, along with glassy carbon (SPI Glas‐22) and silicate glass (NIST SRM 612). Results show that Li content calibration factors (K*) are similar for carbonaceous samples when analysed using a 5 kV secondary ion accelerating voltage. Using a 9 kV secondary ion accelerating voltage,K* factors are negatively correlated with the sample O content, changing ~ 30% between 0 and 15 oxygen atomic %. Thus, to avoid the matrix effect related to O content, using a 5 kV secondary ion accelerating voltage is best for quantification of Li contents based on⁷Li⁺/¹²C⁺ratios. Under these analytical conditions, Li ppm (atomic) = (132 (± 8) × ⁷Li⁺/¹²C⁺) × ¹²C atom fraction of the sample measured. Lithium isotope ratio measurements of SPI Glas‐22 and NIST SRM 612 are within uncertainty; however, the organic polymer samples as a group show a 10‰ higher δ⁷Li than NIST SRM 612.