粉末压片-波长色散X射线荧光光谱法测定金矿型构造叠加晕样品中18种次量元素

金矿床型构造叠加晕样品中的砷锑铋银锡钨等金属元素含量对金矿多期次多阶段成矿具有指示意义。此类样品采集于金矿中,样品各元素含量范围大,从克吨级至百分之几,分布也不均匀。采用常规的检测方法分析时,存在元素间干扰不易消除、记忆效应严重等问题。本文建立了粉末压片-波长色散X射线荧光光谱法测定金矿型构造叠加晕样品中砷锑铋等18种次量元素的定量分析方法。通过研究角度扫描图,选择了干扰少、强度高的分析线;充分混匀样品,消除了偏析效应;选用与样品基体类似的国家标准样品建立工作曲线,通过数学校正和内标法校正了谱线重叠干扰和基体效应。方法检出限为0. 14～2. 23μg/g,精密度(RSD,n=12)小于4%。本方法可快速、准确地测定金矿床型构造叠加晕样品中各元素的含量。     

Rapid Determination of Trace and Ultra Trace Level Elements in Diverse Silicate Rocks in Pressed Powder Pellet Targets by LA‐ICP‐MS using a Matrix‐Independent Protocol

A simple, single sample preparation involving pressed rock powder pellets was utilised to determine the trace and ultra trace abundances of petrogenetically important elements including high field‐strength elements and REEs by laser ablation‐ICP‐MS. One of the elements predetermined by XRF spectrometry served as an internal standard. The influence of sample preparation parameters (grain size, pellet compactness and amount of binding media) on analytical performance was also investigated, including sample homogeneity issues at the laser sampling scale. Line scanning with a high repetition frequency (20 Hz) and large beam diameter (200 μm) ensured ablation from a larger sample surface area, eliminating issues related to sample heterogeneity. A median grain size of about 10 μm for silicate rock powders was found to be sufficiently representative at this scale of laser sampling. Granitic rocks or samples containing resistant minerals such as zircon needed extra grinding to achieve grain sizes down to < 5 μm for better precision for elements that are concentrated in these phases. Using ¹³⁷Ba as an internal standard, reasonable accuracies within 15–20% for most of the high mass trace elements were achieved; in the case of low mass elements, it may deviate up to 40%. Precision of measurements rarely exceeded 15% RSD.     

The contribution of various types of settling particles to the flux of organic carbon in the Gulf of St. Lawrence

The contents of 31 samples from free-drifting sediment traps deployed in the Gulf of St. Lawrence (GSL) were analyzed for the individual contribution of the different types of particles encountered to the total particulate organic carbon (POC) flux. Two trap models were used in 1993-1994: small traps at 50 m depth and large traps at 50 and 150 m. Total POC fluxes averaged 42 mg C m⁻² d⁻¹ for the more reliable large trap and 149 mg C m⁻² d⁻¹ for the small trap. The POC fluxes were attributed to different classes of particles based upon microscopically determined particle dimensions and carbon/volume algorithms available in the literature. Fecal pellets, followed by phytoplankton, were the major attributable components, with important contributions by microzooplankton, particularly during the summer of 1994. The mean fluxes for pellets (6 and 60 mg  C m⁻² d⁻¹, for the large and small traps, respectively) and phytoplankton (3.2 and 42.9 mg C m⁻² d⁻¹) were in the range of those encountered in other areas of moderate primary productivity. Mean zooplankton carbon fluxes (1.8 and 8.5 mg C m⁻² d⁻¹, respectively), however, reflect higher than average zooplankton abundances in the GSL. The C fluxes of specific algal groups confirmed the existence of three trophic regimes previously identified from water column studies and numeric cell fluxes: (1) a period when diatoms were dominant during the spring, (2) a longer interval, which was dominated by dinoflagellates at most others times of the year, and (3) a period of transition during summer. Carbon of animal origin dominated the attributable flux, including an important fraction associated with heterotrophic dinoflagellates. The contribution of marine snow to the total flux (estimated as the difference between the total POC flux and the sum of the attributed components) frequently amounted to more than 60%. The true importance of marine snow remains uncertain, however, because the errors associated with each of the measured components accumulate to produce large uncertainties. The methodological problems involved are discussed.