Determination of Nb and Ta in Nb/Ta minerals by inductively coupled plasmas optical emission spectrometry using slurry sample introduction

The determination of Nb and Ta in Nb-Ta minerals was accomplished by slurry nebulization inductively coupled plasma optical emission spectrometry (ICP-OES), using a clog-free V-groove ceramic nebulizer. Samples were first wet-ground to appropriate particle sizes with narrow size distribution and 90% of the particles in the slurry were smaller than 2.32 mu m in diameter. Subsamples were then dispersed in pH 9 aqueous solutions, and agitated in an ultrasonic bath for 15 min prior to analysis. Due to the lack of slurry standards matching well with the samples, calibration was simply carried out using aqueous solution standards. Results were compared with those obtained from a conventional fusion decomposition procedure and acid digestion procedures and a good agreement between the measured and referred values was obtained. The technique provided a good alternative for the rapid determination of Nb and/or Ta in their corresponding minerals.

Mineralogy of smectites in the surface sediments from the East Pacific and its significance

XRD, TEM, SEM and EDS are employed to analyze smectites in the clay fraction of the surface sediments from the East Pacific. It is shown from the XRD results that the clay fraction consists of about 20% smectites. Three types of smectites are identified, Fe-rich (Type I), Fe, Mg-rich (Type II) and Na,Ca smectite (Type III), and most of them are not well-crystallized. Type I is widely distributed in sediments, showing honeycomblike in the SEM, and aggregated or dispersive hairlike, or cloudy assemblage with a bit curl near its edge in the TEM. This type is considered to be typomorphic type of authigenic smectite in the East Pacific. Type II is similar to Type I in micromorphology in the TEM, showing a transition micronite, while Type III is tabletlike in the TEM with an unclear edge. Type I may be altered from volcanics and some of them even precipitated from the low subthermal water. Type II could also be formed in the ocean floor, while Type III comes from dry and distant continental area. This study suggests that the characteristic of chemical composition and morphology of smectite may give a clue to understand sediment source, origin of minerals and sedimentation in the deep sea.