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对于黑色页岩中的铂钯元素,试样经过灼烧除去硫以及有机质后,用王水分解,经树脂富集,再将树脂灰化后溶解,采用电感耦合等离子体质谱仪测量,取代比色法,得到了更好的检出限,以及准确度。 相似文献
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Determination of total sulfur in geothermal water by inductively coupled plasma-atomic emission spectrometry 下载免费PDF全文
Sulfur speciation and concentration in geothermal water are of great significance for the research and utilization of the water resources. In most situations, it is necessary to determine the total sulfur in geothermal water. In this study, the method was established for the determination of determining total sulfur content — the inductively coupled plasma-atomic emission spectrometry (ICP-AES), with the wavelength of 182.034 nm selected in spectral line of sulfur. It was identified that the optimal working conditions of the ICP-AES instrument were 1 200 W for high frequency generator power 9 mm for vertical observation height, 0.30 MPa atomizer pressure, and 50 r/min analytical pump speed. The matrix interference of the method was eliminated by the matrix matching method. Using this method, sulfur detection limit and minimum quantitative detection limit were 0.028 mg/L and 0.110 mg/L, respectively, whilst the linear range was 0.0–100.0 mg/L. The recovery rate of sample was between 90.67% and 108.7%, and the relative standard deviation (RSD) was between 0.36% and 2.14%. The method was used to analyze the actual samples and the results were basically consistent with the industry standard method. With high analysis efficiency, the method has low detection limit and minimum quantitative detection limit, wide linear range, good precision and accuracy, and provides an important detection method for the determination of total sulfur in geothermal water. 相似文献
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植物样品经逆王水体系微波消解稀释至一定体积后,直接用高分辨等离子体质谱法(HR-ICP-MS)同时测定溶液中的Cr、Mn、Co、Ni、Cu、Zn、As、Se、Mo、Cd、Hg、Pb共12种无机元素的含量。在HR-ICP-MS仪上优化选择各元素的同位素、分辨率和内标元素,有效消除测定过程中的质谱与非质谱干扰。其中,各元素的检出限在0.55~48.6 ng/g之间 (稀释因子=250) ,相对标准偏差RSD(n=12) 均<10%。该方法经国家一级生物标准物质验证,测定结果接近标准值,方法准确可靠,适用于快速准确测定植物样品中的12种元素。 相似文献
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电感耦合等离子体质谱法(ICP-MS)测定水系沉积物中的铌钽锆铪 总被引:1,自引:0,他引:1
建立电感耦合等离子体质谱法(ICP-MS)测定水系沉积物中铌、钽、锆、铪四种元素的分析方法。将样品与氢氧化钠、过氧化钠混合物放入高温炉中,熔融分解完全,用热水提取,过滤后弃去滤液,将滤纸及沉淀用酒石酸-盐酸溶液溶解,稀释至刻度测定。方法检出限(3s)为:LD(Nb)=0.08μg/g,LD(Ta)=0.04μg/g,LD(Zr)=0.5μg/g,LD(Hf)=0.04μg/g,精密度(RSD%,n=6)为:0.84%~4.21%。该测定方法具有灵敏度高、精密度好、分析速度快、线性范围宽、操作性强等优势。采用该方法对国家一级标准物质进行测定表明,其结果与标准值吻合。此方法已在实际地质调查样品分析中得到应用。 相似文献
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Joel BakerDavid Ulfbeck 《Geochimica et cosmochimica acta》2002,66(20):3635-3646
A method has been developed for the rapid chemical separation and highly reproducible analysis of the rare earth elements (REE) by isotope dilution analysis by means of a multiple collector inductively coupled plasma mass spectrometer (MC-ICP-MS). This technique is superior in terms of the analytical reproducibility or rapidity of analysis compared with quadrupole ICP-MS or with thermal ionization mass spectrometric isotope dilution techniques. Samples are digested by standard hydrofluoric-nitric acid-based techniques and spiked with two mixed spikes. The bulk REE are separated from the sample on a cation exchange column, collecting the middle-heavy and light REE as two groups, which provides a middle-heavy REE cut with sufficient separation of the light from the heavier REE to render oxide interferences trivial, and a Ba-free light REE cut. The heavy (Er-Lu), middle (Eu-Gd), and light REE (La-Eu) concentrations are determined by three short (1 to 2 min) analyses with a CETAC Aridus desolvating nebulizer introduction system. Replicate digestions of international rock standards demonstrate that concentrations can be reproduced to <1%, which reflects weighing errors during digestion and aliquotting as inter-REE ratios reproduce to ≤0.2% (2 SD). Eu and Ce anomalies reproduce to <0.15%. In addition to determining the concentrations of polyisotopic REE by isotope dilution analysis, the concentration of monoisotopic Pr can be measured during the light REE isotope dilution run, by reference to Pr/Ce and Pr/Nd ratios measured in a REE standard solution. Pr concentrations determined in this way reproduce to <1%, and Pr/REE ratios reproduce to <0.4%. Ce anomalies calculated with La and Pr also reproduce to <0.15% (2 SD). The precise Ce (and Eu) anomaly measurements should allow greater use of these features in studying the recycling of materials with these anomalies into the mantle, or redox-induced effects on the REE during recycling and dehydration of oceanic lithosphere, partial melting, metamorphism, alteration, or sedimentation processes. Moreover, this technique consumes very small amounts (subnanograms) of the REE and will allow precise REE determinations to be made on much smaller samples than hitherto possible. 相似文献
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Natural variations of Se isotopic composition determined by hydride generation multiple collector inductively coupled plasma mass spectrometry 总被引:1,自引:0,他引:1
Olivier Rouxel John LuddenJean Carignan Luc MarinYves Fouquet 《Geochimica et cosmochimica acta》2002,66(18):3191-3199
Multiple-collector inductively coupled plasma mass spectrometry has been used for the precise measurement of the isotopic composition of Se in geological samples. Se is chemically purified before analysis by using cotton impregnated with thioglycollic acid. This preconcentration step is required for the removal of matrix-interfering elements for hydride generation, such as transitional metals, and also for the quantitative separation of other hydride-forming elements, such as Ge, Sb, and As. The analyte is introduced in the plasma torch with a continuous-flow hydride generation system. Instrumental mass fractionation is corrected with a “standard-sample bracketing” approach. By use of this new technique, the minimum Se required per analysis is lowered to 10 ng, which is one order of magnitude less than the amount needed for the N-TIMS technique. The estimated external precision calculated for the 82Se/76Se isotope ratio is 0.25‰ (2σ), and the data are reported as delta notation (‰) relative to our internal standard (MERCK elemental standard solution). Measurements of Se isotopes are presented for samples of standard solutions and geological reference materials, such as silicate rocks, soils, and sediments. The Se isotopic composition of selected terrestrial and extraterrestrial materials are also presented. An overall Se isotope variation of 8‰ has been observed, suggesting that Se isotopes fractionate readily and are extremely useful tracers of natural processes. 相似文献
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The determination of rare earth elements (REEs), Th and U in seaweeds of various species and in ambient surface seawater were performed by inductively coupled plasma mass spectrometry. The seaweeds and the seawater samples were collected at 10 different coastal areas of Niigata Prefecture in Japan twice a year (spring and autumn) in 2004 and 2005. Results showed that concentration of REEs in seaweed species from Niigata Prefecture were about 103 times higher than those in seawater, and the enrichment factors of REEs were larger in heavy REE than light REE. A significant concentration difference of REEs, Th and U was found among species even in the same phylum. Undaria pinnatifida had the highest concentration of U. Considering that U. pinnatifida has low concentrations of REEs among typical brown algae, different REEs and U uptake mechanisms are suggested. The concentration of REEs, Th and U did not vary remarkably between sampling points and/or seasons. 相似文献
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Synthesis of PGE sulfide standards for laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) 总被引:1,自引:0,他引:1
Cora C. Wohlgemuth-Ueberwasser Chris Ballhaus Jasper Berndt Vaida Stotter née Paliulionyte Thomas Meisel 《Contributions to Mineralogy and Petrology》2007,154(5):607-617
Sulfide compositions with known Re, Os, Ir, Ru, Rh, Pt, and Pd contents are synthesized to be used as standards for noble
metal analysis in solid solution in sulfides. Major elements were added as metals and elemental S. The noble metals, i.e.
35 and 60 ppm each, were added as solutions by micro syringe. Following synthesis at 1 atm the sulfides were sintered at 1.5
to 2 GPa to obtain pellets with theoretical density. Aliquots of the pellets were analysed by isotope dilution ICP-MS for
bulk Re and platinum-group elements (PGE). The spatial noble metal distribution was investigated with an ArF excimer laser
coupled to a single collector ICP mass spectrometer. Sample homogeneity is shown to depend on the metal/S spectrum and the
major element composition of the sulfide, as well as on more subtle factors like oxygen partial pressure during synthesis,
run temperature, and degree of partial melting. The most homogeneous sulfide composition is a (Fe,Ni)1 − x
S monosulfide with 5 wt % Ni and 1-sigma variations in 34S-normalized noble metal count rates of <3.6%. Nearly as homogeneous is a pure Fe1 − x
S monosulfide with 1-sigma variations in 34S-normalized noble metal count rates of <5.8 %. A Cu-bearing Fe1 − x
S monosulfide with 2 wt % Cu was found to be considerably more heterogeneous, suggesting that Cu in solid solution in monosulfides
promotes noble metal heterogeneity. The sulfide composition least suitable for the synthesis of noble metal sulfide standards
is NiS. 相似文献
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电感耦合等离子体质谱法和原子发射光谱法(ICP-MS和ICP-OES)是释光或ESR测年中测定放射性元素含量的常见方法,其样品的预处理是保证测量结果准确的重要环节。本研究通过对8个国家标准沉积物样品(GSS-1a~8a)不同灰化温度后加氢氟酸和硝酸进行预处理,以187Re作为ICP-MS测定时的内标元素,测定U和Th元素,ICP-OES测定K元素。结果表明,相对于350 ℃和450 ℃的灰化温度,550 ℃灰化温度对沉积物中有机质的去除更为彻底,且测定结果的精密度(RSD < 1.3 %)和稳定性更好。将干灰化法(550 ℃)-氢氟酸-硝酸消解体系与常见4种不同湿法消解体系(双氧水-氢氟酸-硝酸、盐酸-氢氟酸-硝酸、王水-逆王水-氢氟酸-硝酸和双氧水-盐酸-氢氟酸-硝酸)对标准沉积物消解后,ICP-MS测定U、Th和ICP-OES测定K元素,干灰化法-氢氟酸-硝酸、盐酸-氢氟酸-硝酸和双氧水-盐酸-氢氟酸-硝酸消解体系下,U、Th和K元素的结果在误差范围内基本一致。进一步将3种消解方式应用于大九湖的15个沉积物样品,结果表明,对于烧失量大于10 % 的样品,盐酸-氢氟酸-硝酸和双氧水-盐酸-氢氟酸-硝酸消解体系下,由于无法完全消解沉积物中全部有机质,导致测定的U、Th和K元素有所偏低。但是沉积物经过干灰化法(550 ℃)处理后,样品极易溶解,消解液透亮无杂质,且加酸量少,对沉积物中U、Th和K元素的测定结果更为稳定。这一结果揭示干灰化法-氢氟酸-硝酸消解体系适宜于对大批量第四纪沉积物样品U、Th和K元素的光谱-质谱联用技术检测。
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The determination of accurate Sr isotope ratios in calcium phosphate matrices by laser ablation multi-collector ICP-MS is demonstrated as possible even with low Sr concentration archaeological material. Multiple on-line interference correction routines for doubly-charged REE, Ca dimers and Rb with additional calibration against TIMS-characterised materials are required to achieve this. The calibration strategy proposed uses both inorganic and biogenic apatite matrices to monitor and correct for a 40Ca-31P-16O polyatomic present at levels of 0.3-1% of the non-oxide peak, which interferes on 87Sr causing inaccuracies of 0.03-0.4% in the 87Sr/86Sr isotope ratio. The possibility also exists for synthetic materials to be used in this calibration. After correction for interferences total combined uncertainties of 0.04-0.15% (2SD) are achieved for analyses of 13-24 μg of archaeological tooth enamel with Sr concentrations of ca. 100-500 ppm using MC-ICP-MS. In particular, for samples containing >300 ppm Sr, total uncertainties of ∼0.05% are possible utilising 7-12 ng Sr. Data quality is monitored by determination of 84Sr/86Sr ratios.When applied to an archaeological cattle tooth this approach shows Sr-isotope variations along the length of the tooth in agreement with independent TIMS data. The 40Ca-31P-16O polyatomic interference is the root cause of the bias at mass 87 during laser ablation ICP-MS analysis of inorganic and biogenic calcium phosphate (apatite) matrices. This results in inaccurate 87Sr/86Sr ratios even after correction of Ca dimers and doubly charged rare earth elements. This interference is essentially constant at specific ablation conditions and therefore the effect on 87Sr/86Sr data varies in proportion to changes in the Sr concentration of the ablated material. Complete elimination of this interference is unlikely through normal analytical mechanisms and therefore represents a limitation on the achievable accuracy of LA-(MC-)ICP-MS 87Sr/86Sr data without rigorous calibration to known reference materials. 相似文献
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本文介绍了电感耦合等离子体发射光谱法测定生物样品中Fe、Ca、Mg、K、Na、P等元素的分析方法,参加了国家植物标准物质定值,结果令人满意。 相似文献