氨基羧酸纤维分离富集-电感耦合等离子体原子发射光谱法测定多种痕量稀土元素

本文制备了氨基羧酸纤维滤纸片作为柱填充物，成功地分离和富集了地化样品中的多种稀土元素。富集后的稀土元素采用电感耦合等离子体原子发射光谱法测定，回收率为90％～109％。本文还对基体干扰及其消除进行了研究。     

共沉淀分离富集-电感耦合等离子体原子发射光谱法测定高纯氧化钨中痕量金属杂质

提出了以Ｌａ（ＯＨ）３为共沉淀剂，对高纯氧化钨中的痕量金属杂质元素经共沉淀预分离富集后进行ＩＣＰ－ＡＥＳ测定的分析方法。探讨了影响杂质元素回收率和钨残留量的若干因素，确定了合适的分离富集条件。合成试样和标准样品的测试结果表明： Ｂｉ、Ｃａ、Ｃｄ、Ｃｏ、Ｃｕ、Ｆｅ、Ｍｇ、Ｍｎ、Ｎｉ、Ｐｂ、Ｓｂ、Ｓｎ、Ｔｉ等元素能被定量分离回收，回收率和精密度均令人满意。     

两性离子交换纤维柱富集-电感耦合等离子体原子发射光谱法测定水样中稀土元素

提出了两性离子交换纤维柱吸附富集镧、钕、铕、钆、铒和镱,1.5mol·L~(-1)硝酸溶液作洗脱剂,电感耦合等离子体原子发射光谱法测定水样中上述痕量稀土元素含量的方法。在优化的试验条件下,两性离子交换纤维柱对镧、钕、铕、钆、铒和镱的吸附容量分别为7.32,7.61,8.04,7.95,9.12,8.49 mg·g~(-1);镧、钕、铕、钆、铒和镱的检出限(3S/N)分别为0.032,0.068,0.033,0.053,0.045,0.019μg(-1)。方法用于水样中镧、钕、铕、钆、铒和镱含量的测定,回收率在90.0%～101.0%之间,相对标准偏差(n=5)在1.7%～5.4%之间。     

流动注射-氢化物发生-电感耦合等离子体原子发射光谱法测定铜合金中痕量砷

本文研究了732强酸性阳离子交换树脂对铜离子的交换条件,并与流动注射(FⅠ)相结合,建立了一种新型高效的在线FⅠ-阳离子交换-氢化物发生-ICP-AES分析体系。本法经离子交换柱可消除高达10mg/ml铜离子的干扰,同时可以使分析速度和灵敏度大大提高。每小时可分析25个样品,砷的检出限为0.9μg/g。     

萃取分离电感耦合等离子体原子发射光谱法测定钢中的微量稀土元素

本文采用苯甲酰苯胲(BPHA)-甲基异丁基酮(MIBK)溶剂萃取方法将钢中基体元素Fe,Ti,Mo,V等大量非稀土元素萃入有机相中,稀土元素留于水溶液中.由电感耦合等离子体原子发射光谱(ICP-AES)仪直接测定水溶液中的微量稀土元素La,Ce,Pr,Nd.Sm,Y和Gd,实验结果与推荐值基本相符,方法的回收率为96％～108％,相对标准偏差低于5％.     

碱性氯化法破氰-碲共沉淀富集-电感耦合等离子体原子发射光谱法测定氰化退镀液中金含量

采用碱性氯化法氧化分解样品中氰化物,碲共沉淀法分离富集破氰溶液中的金,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定退镀液中金的分析方法. 在碱性条件下,使用次氯酸钠氧化分解退镀液中的氰化物,使其转化为二氧化碳和氮气,使用亚硫酸钠溶液中和破氰溶液中的余氯,消除氧化物对氰化物测试包的影响,可以简便快速判断退镀溶液破氰效果. 在3.6 mol/L盐酸介质中,12.5 mL碲溶液(2.5 g/L)和11.0 mL氯化亚锡溶液(1 mol/L)可定量沉淀5~500 μg金,50倍量的杂质元素不干扰测定. 金的质量浓度在0.05~25.00 mg/L范围内与其发射强度呈线性,线性回归方程为y=46.487x+0.343,相关系数r大于0.999 9,检出限为0.004 4 mg/L. 对实际样品进行准确度考察,测定结果的相对标准偏差(RSD, n=7)低于1.0%,加标回收率为96.9%~103.1%,实际样品测定结果与火试金法的对照结果一致性好.     

电感耦合等离子体原子发射光谱法测定某些特殊试样中痕量铬(Ⅵ)——共沉淀法快速分离铬(Ⅲ)

电感耦合等离子体原子发射光谱法(ICP-AES)应用于某些特殊试样(特别试液背景色泽很深或略带混浊者)中铬(Ⅵ)的测定.试样溶液中共存的铬(Ⅲ)及一些其他金属离子的干扰,借在PH 9.5的氨性溶液中以Fe(Ⅲ)离子作载体共沉淀分离予以消除,用ICP-AES法测定滤液中铬(Ⅳ).试验表明:铬(Ⅲ)共存量达100 mg·L-1时,经沉淀分离后不影响铬(Ⅵ)的测定,铬(Ⅵ)的回收率接近100%.此方法的检出限(3σ)为0.054 mg·L-1,应用所提出的方法测定了一种黄色油漆中在铬(Ⅲ)共存下的铬(Ⅵ),平行7次测定,相对标准偏差为1.3%.     

纳米氧化铝微柱富集-等离子体发射光谱法测定植物中痕量稀土元素

以负载了1-苯基-3-甲基-4-苯甲酰基-吡唑酮[5](PMBP)的纳米氧化铝为微柱吸附材料，采用等离子体原子发射光谱法(ICP-AES)，系统地研究了其在动态条件下对稀土离子Sc^3 、Y^3 和La^3 的吸附性能，并确定了最佳吸附及解脱条件。实验结果表明：在pH为4．5时，分析物均可被上述吸附材料定量吸附；用0．5moL／L盐酸溶液可将吸附在微柱上的稀土离子完全解脱。本法对Sc^3 、Y^3 和La^3 的检出限分别为0．16、0.19和0．39μg／L；相对标准偏差(RSD)分别为2．7％、3．2％和1．6％(n=9，C=0．5mg／L)。方法应用于植物标样中痕量Sc、Y和La的测定，其测定值与标样值吻合很好。     

电感耦合等离子体原子发射光谱法测定高纯氧化钇铕中13种杂质稀土元素

采用电感耦合等离子体原子发射光谱法(ICP-AES)测定了高纯氧化钇铕中13种杂质稀土元素。取样品1.000 0 g溶于盐酸10 mL中,加水定容至100 mL,供ICP-AES分析,选定了所测定的13种杂质稀土元素的分析谱线。测定中所选用的仪器工作参数为:①冷却气流量12 L.min-1;②护套气流量0.20 L.min-1;③载气流量3.0 L.min-1;④高频发生器频率40.68 MHz,功率1.1 kW;⑤观测高度10～12 mm。用标准加入法对方法的回收率及精密度作了试验,所得回收率在78.5%～99.6%之间;测定值的相对标准偏差(n=11)在0.02%～0.94%之间。     

Inductively coupled plasma atomic emission spectrometric determination of 27 trace elements in table salts after coprecipitation with indium phosphate

The coprecipitation method using indium phosphate as a new coprecipitant has been developed for the separation of trace elements in table salts prior to their determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). Indium phosphate could quantitatively coprecipitate 27 trace elements, namely, Be, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd, Pb, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, in a table salt solution at pH 10. The rapid coprecipitation technique, in which complete recovery of the precipitate was not required in the precipitate-separation process, was completely applicable, and, therefore, the operation for the coprecipitation was quite simple. The coprecipitated elements could be determined accurately and precisely by ICP-AES using indium as an internal standard element after dissolution of the precipitate with 5 mL of 1 mol L⁻¹ nitric acid. The detection limits (three times the standard deviation of the blank values, n = 10) ranged from 0.001 μg (Lu) to 0.11 μg (Zn) in 300 mL of a 10% (w/v) table salt solution. The method proposed here could be applied to the analyses of commercially available table salts.     

Flow injection on-line preconcentration with an ion-exchange resin coupled with microwave plasma torch-atomic emission spectrometry for the determination of trace rare earth elements

A sensitive and rapid on-line method has been developed for the determination of trace amounts rare earth elements (REEs), lanthanum, cerium, neodymium and yttrium, by microwave plasma torch-atomic emission spectrometry (MPT-AES) combined with micro-column separation/preconcentration. A strong basic cinnamene anion exchange resin is used for matrix elimination and enrichment of the analytes. The adsorbed metal ions are subsequently eluted from the column and transferred into the detector with nitric acid solution for simultaneous multi-element determination. Various factors influencing the separation/preconcentration, sample flow rate, loading time, acidity and eluent flow rate, concentration, have been studied in detail. Under the optimized conditions, the detection limits for lanthanum, cerium, neodymium and yttrium based on three times of standard deviations of blank by 7 replicates are 0.89, 2.02, 1.56 and 0.78 μg·L^− 1, and the relative standard deviations are determined as 1.54, 4.29, 4.95 and 3.90%, respectively. The proposed method has been applied to the analysis of the four REEs in high purity Sm₂O₃, Eu₂O₃, Gd₂O₃, Tb₂O₃, Dy₂O₃, Yb₂O₃, and Lu₂O₃ samples with a recovery range of 95.1-104.8%.     

Preconcentration and atomic spectrometric determination of rare earth elements (REEs) in natural water samples by inductively coupled plasma atomic emission spectrometry

The usage of a variety of sorbents has been shown as promising matrix removal/preconcentration strategies for the determination of rare earth elements (REEs) in various natural water samples by inductively coupled plasma atomic emission spectrometry (ICP-AES). The sorption efficiency of various zeolites (clinoptilolite, mordenite, zeolite Y, zeolite Beta), ion-exchangers (Amberlite CG-120, Amberlite IR-120, Rexyn 101, Dowex 50W X18) and chelating resins (Muromac, Chelex 100, Amberlite IRC-718) towards REEs was investigated in terms of solution pH, shaking time and sorbent amount. The results have shown that most of the materials can take up REEs at a wide pH range. The experiments were continued with clinoptilolite, zeolite Y and Chelex 100 and it was demonstrated that all three materials displayed very fast kinetics for REE sorption (higher than 96% in 1 min). Desorption from the sorbents was realized with 2.0 M HNO₃ for clinoptilolite and 0.1 M HNO₃ for zeolite Y and Chelex 100. Only the lower concentration range (0.01-2.0 mg l⁻¹) of matrix-matched standards were used in quantitation although the calibration graphs were linear at least up to 10.0 mg l⁻¹ for all REEs studied. The limit of detection (3 s) without preconcentration was 0.1, 1.0, and 0.2 μg l⁻¹ for Eu, La, and Yb, respectively. The validity of the method with the selected sorbents was checked through spike recovery experiments.     

Determination of trace elements in human serum by inductively coupled plasma atomic emission spectrometry with flow injection

An analytical method for the simultaneous determination of some trace elements (Au, Fe, Mg, Li, Sr, Zn) in human serum by inductively coupled plasma atomic emission spectrometry (ICP-AES) with flow injection is described. Physical interference caused by the change of sample viscosity is discussed. When 100 μl of serum was injected, the relevant recoveries of > 99% for Li, > 98% for Cu and Mg, > 95% for Fe were obtained for an NIST SRM with R.S.D. > 1.3% using optimized flow injection parameters. The prepared lyophilized control serum for routine analysis in clinical laboratories was analyzed and verified for the validity of the technique employed in this experiment using NIST SRM 909 as a primary reference material.     

ICP-AES 法测定硅铁中痕量元素

采用电感耦合等离子原子发射光谱法测定硅铁中的痕量元素,研究了 Fe 基体对被测元素的影响,并选择了最佳工作条件.被测元素的检测限为 0 .60～76.2 ng/mL,样品加标回收率为 92%～108%,RSD(n=8)<3%.     

电感耦合等离子体原子发射光谱法（ICP-AES）测定RoHS指令聚合物中的铅和镉

本文引入微波技术消解聚合物塑料样品,使用电感耦合等离子体原子发射光谱仪（ICP-AES）测定聚合物中的铅（Pb）和镉（Cd）含量,并建立了优化的样品消解程序和测定方法,得到满意的测定结果。[摘要应包括目的、方法、结果、结论,请修改,同时修改英文]该方法具有效率高、污染小的优点。检测结果具有良好的精密度。     

Inductively coupled plasma optical emission spectrometric determination of trace elements in sediments after sequential selective extraction: effects of reagents and major elements on the analytical signal

The interfering effects due to the reagents and matrix elements associated with a four step sequential extraction procedure on ICPOES determination of trace elements were investigated in a systematic way. The emission lines were selected in order to include the most interesting elements for environmental studies (Zn, Pb, Ni, Cr, V and Cu) and the concentrations ranged according with the values occurring in the real samples. In order to distinguish between chemical and physical interfering effects, the Mg 280.270–Mg 285.213 line intensity ratio was measured, in each condition. Both pneumatic and ultrasonic nebulization were considered for comparison. It was found that both the elements which constitute the sample and the reagents which are added during the sample preparation steps significantly influence the emission intensity of all the analytes, depending on the analytical concentration and the nebulization system. Generally, the signal variations were higher with ultrasonic nebulization. Concerning the interference mechanism, it was found that the effect of the major elements (Na, K, Mg, Ca, Al and Fe) is essentially related to a change of the aerosol generation and transport processes. Differently, acetic acid, ammonium acetate and hydroxylamine hydrochloride significantly improved the plasma excitation conditions, depending on their concentration. A change of the sample introduction efficiency due to the presence of these reagents was also evident. On the contrary, the effect of hydrochloric and nitric acid emerged to be related only to the processes occurring in the sample introduction system.     

Inductively coupled plasma optical emission spectrometric determination of trace element in PM10 airborne particulate matter collected in an industrial area of Argentina

Trace metals of relevance from the environmental and toxicological point of view were quantified in the city of Campana, Buenos Aires, Argentina. The collection of particulate matter was performed on ash-free fiber glass filters using high-volume samplers with a PM₁₀ sampling head, during a 3-month period in 2002. An acid leaching of elements deposited on the filters was adopted paying special attention to the recovery of volatile elements. Analysis was performed by inductively coupled plasma optical emission spectrometry (ICP OES) to ascertain the concentrations of 12 key elements, namely, Al, As, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Ti, V and Zn. The validation of the procedure was performed by the analysis of the standard reference material NIST 1648, urban particulate matter, and good agreement between concentrations found and the reported certified values was achieved. Blank filters were spiked with the analytes investigated and the recoveries varied between 83% and 92%. Metal concentrations spanned the range 0.03 ng m⁻³ (equivalent to 0.42 μg g⁻¹) for Cd to 1.9 μg m⁻³ (equivalent to 29.7 mg g⁻¹) for Fe. The results obtained show that the pollutants of special environmental and health concern are As and Pb. Mean As concentration was higher than the guideline value associated with an excess cancer risk of 1:10⁻⁶, reported by the World Health Organization (WHO). Lead is the only element that showed higher concentrations than those recently measured in the large and heavily trafficked metropolitan area of Buenos Aires. Cadmium>Pb>As>Zn>Cu are the elements more enriched in airborne PM₁₀.     

Silicon determination by inductively coupled plasma atomic emission spectrometry after generation of volatile silicon tetrafluoride

A method for the determination of silicon by inductively coupled plasma atomic emission spectrometry (ICP-AES) is described. The procedure is based on a discontinuous generation of volatile silicon tetrafluoride in concentrated sulphuric acid medium after injecting 125 μl of 0.1%, w/v sodium fluoride solution into 100 μl of the sample. The gaseous silicon tetrafluoride is fed directly into the ICP torch by a flow of 250 ml min⁻¹ Ar carrier gas. The calibration curve was linear up to at least 100 μg ml⁻¹ of Si(IV) and the absolute detection limit was 9.8 ng working with a solution volume of 100 μl. The relative standard deviation for six measurements of 10 μg ml⁻¹ of Si(IV) was 2.32%. The method was applied to the determination of silicon in water and iron ores.     

Accurate determination of trace amounts of phosphorus in geological samples by inductively coupled plasma atomic emission spectrometry with ion-exchange separation

In order to determine trace amounts of phosphorus in geological and cosmochemical rock samples, simple as well as reliable analytical schemes using an ICP-AES instrument were investigated. A (conventional) ICP-AES procedure could determine phosphorus contents at the level of several 100 μg g⁻¹ with a reasonable reproducibility (<10% for 200 μg g⁻¹; 1σ). An ICP-AES procedure coupled with matrix-separation using cation and anion exchange resins could lower the quantification level down to 1 μg g⁻¹ or even lower under the present experimental conditions. The matrix-separation ICP-AES procedure developed in this study was applied to twenty-one geological reference samples issued by Geological Survey of Japan. Obtained values vary from 1250 μg g⁻¹ for JB-3 (basalt) to 2.07 μg g⁻¹ for JCt-1 (carbonate). Matrix-separation ICP-AES yielded reasonable reproducibility (less than 8.3%; 1σ) of three replicate analyses for all the samples analyzed. In comparison of our data with certificate values as well as literature or reported values, there appear to be an apparent (and large) discrepancy between our values and certificate/reported values regardless of phosphorus contents. Based on the reproducibility of our data and the analytical capability of the matrix-separation ICP-AES procedure developed in this study (in terms of quantification limit, recovery, selectivity of an analyte through pre-concentration process, etc.), it is concluded that certified values for several reference standard rocks should be reevaluated and revised accordingly. It may be further pointed that some phosphorus data reported in literatures should be critically evaluated when they are to be referred in later publications.