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1.
本文报道用HNO3-H2O2微波溶样,不经分离富集,用标准加入ICP-MS法,直接测定茶叶中15种痕量稀土元素,对微波溶样和等离子体质谱测定条件进行了优化选择,在最佳实验条件下,用本法测定了国家一级茶叶标准GBW07605中的单一稀土元素,测得值与标准值很好吻合。 相似文献
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本文采用微波溶样,不经分离富集,直接用标准加入ICP-MS法,测定人发标准物质中15种超痕量稀土元素。选择了最佳样品预处理条件和测定的最佳仪器参数。检出限为0.007~0.026ng/mL。用国家一级土壤标准物质(GBW07401和GBW07403)作为质控样,15种痕量稀土元素的测得值与标准值很好地吻合,相对标准偏差(RSD)为1.2%~5.4%。国家一级人发标准物质(GBW07601)中稀土元素的标准值仅有La,Ce和Y,本法测得值均落在标准值的置信区间内。其余12个超痕量稀土元素本法也取得了较为满意的结果。 相似文献
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微波溶样-分光光度法测定螺旋藻中的碘 总被引:2,自引:0,他引:2
用微波溶样-分光光度法测定螺旋藻中的碘,溶样快速,简单,安全。RSD2.4% ̄4.1%,回收率97.1% ̄103.3%。 相似文献
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微波溶样—ICP—AES法测定人发标准物质中15种超痕量稀土元素的研究 总被引:5,自引:0,他引:5
本文采用微波溶样,不经分离富集,直接用标准加入ICP-MS法,测定人发标准物质15种超痕量稀土。选择了最佳样品预处理条件和测定的最佳仪器参数。 相似文献
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离子色谱法测定α—氧化铝中微量硫酸根的研究 总被引:1,自引:0,他引:1
本建立了用氢氧化钠溶样,离子色谱测定α-Al2O3中微量硫酸根的方法。在DionexAS4A分离柱上,用1.8×10^-^3mol/LAa2CO3作流动相进行洗脱,电导检测器检测,分析方法简便,快速,硫酸根的检测限为1.0×10^-^2μg/ml,相对标准偏差为2.67%,回收率为97.5%,扩展了离子色谱法测定实际样品的范围。 相似文献
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感耦等离子体质谱法(ICP—MS)测定高纯氧化镝中痕量稀土杂质 总被引:1,自引:0,他引:1
本文报道用2-乙基己基膦酸单酯萃淋树脂为固定相,HCl为淋洗液的萃取色谱法研究了高纯Dy2O3中的痕量稀土杂质和Dy2O3基体的分离条件,并用ICP-MS法测定了高纯Dy2O3中的14个稀土杂质,稀土元素的测定限为0.001-0.005ICP-MS法测定了高纯Dy2O3 相似文献
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原子吸收法在有机分析中的应用(Ⅲ):茶叶中茶多酚的测定 总被引:14,自引:0,他引:14
研究了间接测定茶叶中茶多酚的原子吸收,用甲基异丁酮和丁醇的混合溶剂萃取茶汤中的茶多酚,与氨基酸分离后,加入碱性Cu3(PO4)2悬浮液反萃取并同茶多酚作用,离心沉降未作用的Cu3(PO4)2后,用原子吸收法测定Cu,可求得茶多酚的含量,本法可消除茶叶共存氨基酸的干扰,测定结果同标准方法一致,回收率范围为94%-104%,平均标准偏差为3.1%。 相似文献
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动力学—两次标准加入法同时测定钼和钨 总被引:4,自引:3,他引:4
本文提出了动力学-两次标准加入法双组份同时测定的新方法,讨论了测定的基本原理;用停流FIA光度法研究了钼和钨共同催化的H2O2-I^-动力学反应体系,并建立了钼和钨同时测定的条件,用本法测定了钢样和模拟样品中的钼、钨含量,结果满意,钼和钨的回收率分别为97%-102.6%和98.2%-103%;相对标准偏差分别为2.8%-3.2%和2.1%-3.5%。 相似文献
9.
微波条件下V2O5/TiO2低温选择氧化甲苯制苯甲酸 总被引:13,自引:0,他引:13
在微波辐射条件下,考察了甲苯选择氧化过程中催化剂床层温度、O2/甲苯比、原料气总空速、V2O5担载量和添加氧化物助剂等条件对V2O5/TiO2催化剂活性的影响.结果表明,在微波作用下,当床层温度在250℃,O2/甲苯摩尔比6和原料气总空速10000h-1时,1%MoO3-8%V2O5/TiO2上的苯甲酸和苯甲醛的收率分别达到41%和14%.与传统加热的催化过程相比,苯甲酸和含氧化物的收率均有较大的提高.还初步探讨了微波对催化剂活性的影响. 相似文献
10.
ICP-AES法同时测定石英砂中的痕量元素 总被引:3,自引:0,他引:3
采用微波溶样,并通过条件试验,建立了微波溶样ICP-AES法同时测定石英砂中13种痕量元素的分析方法并已应用于实际样品的分析,方法的相对标准偏差≤10%,加标回收率为90%-107%。 相似文献
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采用1-苯基-3-甲基-4-苯甲酰基-5-吡唑酮(PMBP)苯溶液萃取分离-ICP-AES法同时测定茶叶中15种稀土元素,消除了基体的干扰,并对样品前处理方法、萃取分离条件进行了考查.方法回收率为: 92.3%~112%,相对标准偏差<2.5%.在最佳工作条件下,测定了茶叶标准物质(GBW07605)中稀土元素,结果与标准值吻合. 相似文献
15.
V. Balaram 《Accreditation and quality assurance》2000,5(8):325-330
Under an international collaborative certification programme, two new Polish soil reference materials, PL-1 (loess) and BPGM-1
(sandy loam soil), were analysed for 34 trace elements including all the rare earth elements using the acid decomposition
method and inductively coupled plasma - mass spectrometry (ICP-MS). After the certification by the organisers, the analytical
data obtained at our institute were compared with the certified data. 'Z-score' values calculated for individual trace elements
helped in the assessment of the quality of the data. While the majority of the data obtained on ICP-MS was very precise and
accurate, some of the data especially for elements such as Zr, Hf and Nb suffered from incomplete dissolution of the sample
and spectroscopic interferences. For some trace elements, certified data are not available for comparison. These features
together with the usefulness of interlaboratory collaborative programmes and ICP-MS for the certification of soil reference
materials are discussed.
Received: 6 August 1999 / Accepted: 28 February 2000 相似文献
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《Analytical letters》2012,45(11):2105-2115
Abstract Systematic investigations were carried out into the sorption of rare earth elements (REEs) on carbon nonofibers (CNFs) by inductively coupled plasma mass spectrometry (ICP‐MS). The experimental parameters for preconcentration of REEs, such as pH, sample flow rate and volume, eluent concentration, and interfering ions on preconcentration of REEs have been examined in detail. The studied metal ions can be adsorbed quantitatively on CNFs in a pH range from 2.0 to 5.0, and then eluted completely with 0.5 mol l?1 HNO3. Based on the above facts, a novel method using a microcolumn packed with carbon nanofibers as an adsorption material was developed for the separation and preconcentration of REEs prior to their determination by ICP‐MS. The proposed method has been successfully applied to the determination of light (La), medium (Eu and Gd) and heavy (Yb) rare earth elements in real sample with the recovery more than 90%. In order to validate this method, two certified reference materials of tea leaves (GBW 07605) and mussel (GBW 08571) were analyzed, and the determined values are in good agreement with the certified values. 相似文献
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《Spectrochimica Acta Part B: Atomic Spectroscopy》2005,60(1):125-129
A new method has been developed for the determination of trace rare earth elements (REEs) in water samples based on preconcentration with a microcolumn packed with multiwalled carbon nanotubes (MWNTs) prior to their determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). The optimum experimental parameters for preconcentration of REEs, such as pH of the sample, sample flow rate and volume, elution solution and interfering ions, have been investigated. The studied REEs ions can be quantitatively retained by MWNTs when the pH exceed 3.0, and then eluted completely with 1.0 mol L−1 HNO3. The detection limits of this method for REEs was between 3 and 57 ng L−1, and the relative standard deviations (RSDs) for the determination of REEs at 10 ng mL−1 level were found to be less than 6% when processing 100 mL sample solution. The method was validated using a certified reference material, and has been successfully applied for the determination of trace rare earth elements in lake water and synthetic seawater with satisfactory results. 相似文献
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The influence of matrix elements such as Ba, Ca, Fe, K, Na and Ti, on the inductively coupled plasma atomic emission spectrometry determination of the rare earth elements in soils and sediments is investigated and analytical lines with minimal interferences are chosen. The analysis of certified reference materials by two calibration methods (pure rare earth solutions and IAEA-Soil 5) and after cation-exchange proved that calibrations with IAEA-Soil 5 increase the number of accurately determined rare earth elements (REE), permitting the instrumental determination of Ce, Eu, La, Nd, Tb, Yb and Y in soils and some sediments. The cation-exchange procedure permits the determination of 12 REE with very good accuracy (below 10%) and detection limits varying between 0.05 (Eu, Tb, Yb) and 0.5 (Er) mg kg(-1). 相似文献
20.
Kh. Rezaee M. R. Abdi E. B. Saion K. Naghavi M. A. Shafaei 《Journal of Radioanalytical and Nuclear Chemistry》2011,287(3):733-740
In order to complete having data base of elemental assessment of the east coast of Peninsular Malaysia marine sediments along
the South China Sea coasts, trace elements are analyzed and their distribution in marine sediments is undertaken. The present
study is done parallel with pervious study on elemental assessment of heavy metals, rare earth elements and actinides in the
marine sediments of the east coast of Peninsular Malaysia. Thirty surface sediment samples were collected in this area, including
regions of Kelantan, Terengganu, Pahang, Rompin and Johor Baharu. Multielemental analysis was carried out by instrumental
neutron activation analysis and inductively coupled plasma atomic emission spectroscopy. In both cases methodology validation
was performed by certified reference material analyses. For the surface elemental distributions the enrichment factor values,
average I
geo and mC
d values indicate that the trace elements of the surface sediments are uncontaminated in all sampling stations that are consistent
with previous studies results of heavy metals, rare earth elements and actinides. 相似文献