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We used samples from six Finnish ore deposits to evaluate the efficiency of sample pretreatment procedures — crushing, splitting and grinding — and to compare three analytical methods based on the atomic absorption determination of gold following: (1) classical lead fire assay (FA); (2) the aqua regia leach (AR) followed by Hg coprecipitation of Au; and (3) the sodium cyanide (NaCN) leach. Sample size used for the method comparison is 20 g. The Au deposits and ore types were: Suurikuusikko and Osikonmäki, refractory ores in which Au is associated with arsenopyrite and pyrite; Pampalo and Kutemajärvi ores with metallic Au and Au tellurides; and Jokisivu and Pahtavaara ores containing coarse-grained metallic Au. After crushing, the samples were split into three parts, one of which was put aside into storage. Two splits were further divided into two subsamples which were ground to two grades of fineness (<0.03 and <0.06 mm). The four subsamples thus obtained were analysed for Au using the three analytical methods. Each determination was performed five times on each of the four subsamples. According to t-tests on the FA results of the two splits, crushing and splitting produced samples of equal Au content in all six cases. Grinding to a finer grain size gave a significant difference in Au results only for the Pahtavaara ore sample. If the FA results are assumed to represent 100% recovery of Au, we obtained greater than 95% recoveries for all but the Suurikuusikko sample (87% recovery) by the AR leach method. We also obtained recoveries of over 95% by the NaCN leach method for the Pampalo, Kutemajärvi and Pahtavaara samples, whereas recoveries for the other three samples varied between 73 to 92%. The AR leach was also performed on 1-g samples and the NaCN leach on 250-g samples. For three of the ore samples, decreasing sample size from 20 g to 1 g did not cause a significant difference in the variance of the Au results. Increasing the sample size from 20 g to 250 g significantly improves the representativity of only the Pahtavaara sample. For the Kutemajärvi, Pahtavaara and Jokisivu ores, a sample larger than 250 g is needed in order to obtain a precision equivalent to that for reference samples. 相似文献
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Determination of Trace Element Mass Fractions in Ultramafic Rocks by HR‐ICP‐MS: A Combined Approach Using a Direct Digestion/Dilution Method and Preconcentration by Coprecipitation 
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下载免费PDF全文 Mathieu Rospabé Mathieu Benoit Frédéric Candaudap 《Geostandards and Geoanalytical Research》2018,42(1):115-129
A procedure is described for the determination of thirty‐seven minor and trace elements (LILE, REE, HFSE, U, Th, Pb, transition elements and Ga) in ultramafic rocks. After Tm addition and acid sample digestion, compositions were determined both following a direct digestion/dilution method (without element separation) and after a preconcentration procedure using a double coprecipitation process. Four ultramafic reference materials were investigated to test and validate our procedure (UB‐N, MGL‐GAS [GeoPT12], JP‐1 and DTS‐2B). Results obtained following the preconcentration procedure are in good agreement with previously published work on REE, HFSE, U, Th, Pb and some of the transition elements (Sc, Ti, V). This procedure has two major advantages: (a) it avoids any matrix effect resulting from the high Mg content of peridotite, and (b) it allows the preconcentration of a larger trace element set than with previous methods. Other elements (LILE, other transition elements Cr, Mn, Co, Ni, Cu, Zn, as well as Ga) were not fully coprecipitated with the preconcentration method and could only be accurately determined through the direct digestion/dilution method. 相似文献
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An improvement in the small-volume technique for determining thorium-234 in seawater 总被引：3，自引：0，他引：3
The recently developed 2–5 L small-volume MnO2 coprecipitation method for determining 234Th in seawater has provided a new way to substantially increase, both temporally and spatially, the sampling resolution of 234Th and 234Th-based particulate organic carbon export estimates in the upper ocean. In this study, we further optimize the technique by reducing reagent quantities and the use of an additional water bath heating step. This optimization allows the filtration of the MnO2 precipitate onto a 25-mm diameter, 1.0 μm pore size QMA filter to be completed within < 30 min for unfiltered waters from the South China Sea. In addition, we have modified the MnO2 purification procedure to allow for alpha spectrometric measurements of 234Th recoveries. Results from recovery experiments suggest that reagent amounts can be reduced to 0.0375 mg KMnO4 and 0.1 mg MnCl2·4H2O per liter of sample, while still maintaining high 234Th recovery. This study further confirms that the addition of a yield monitor is necessary for the application of the small-volume method. 相似文献
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We present dissolved load (< 0.45 μm) rare earth element (REE) patterns of small streams from a catchment basin in the Massif Central in order to characterize the individual fractionation stages for the dissolved REE from the source to the catchment outlet. The upper part of the catchment is located on a basalt plateau, followed downstream by deep and narrow valleys with granitic and orthogneissic bedrock. Stream water has basalt-like REE patterns on the basaltic plateau close to the source, followed by a continuous depletion in light REE (La-Sm, LREE) downstream. Strontium and neodymium isotope ratios of stream water demonstrate that the dissolved REE are essentially of basaltic origin, even in the lower, granitic and gneissic part of the catchment. Mixing with gneiss or granite derived REE thus cannot explain the observed evolution of the REE patterns. There seems also to be no link with the calculated speciation of the dissolved REE. In contrast, a correlation between saturation indexes for hematite and La/Yb ratios suggests that REE fractionation is mainly controlled by precipitation of Fe-oxide particles that preferentially remove LREE from solution. 相似文献