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1.
本工作通过比较端视与侧视ICP的分析性能,研究了端视ICP系统对稀土元素的分析特性。高频发生器输出功率与载气流量对端视与侧视ICP激发特性的影响没有明显差异,取光方式的不同是二者分析性能差异的根本原因。端视ICP由于取光时避开了产生连续背景的环形热区和截取了整个中心通道的光谱.其背景减小,谱线强度增强,获得较好的测定下限。对14种稀土元素测定下限的比较表明:端视ICP比铡视ICP下降10-30倍。 相似文献
2.
本工作通过比较端视与侧视ICP的分析性能,研究了端视ICP系统对稀土元素的分析特性。高频发生器输出功率与载气流量对端视与侧视ICP激发特性的影响没有明显差异,取光方式的不同是二者分析性能差异的根本原因。端视ICP由于取光时避开了产生连续背景的环形热区和截取了整个中心通道的光谱,其背景减小,谱线强度增强,获得较好的测定下限。对14种稀土元素测定下限的比较表明:端视ICP比铡视ICP下降10-30倍。 相似文献
3.
ICP—AES中基体及操作条件对元素电离度的影响 总被引:2,自引:0,他引:2
本文测定了Ca、Cd、Mg、Mn、Zn5种元素电离度在1CP中的垂直空间分布,观察了基体元素及操作条件(正向功率与载气流量)对电离度的影响,结果表明,元素的电离度与ICP的激发特性没有直接的联系;基体元素及操作条件对电离度影响很小。 相似文献
4.
采用ICP—AES法同时测定黑豆和红小豆中Na,Sn,Ca,Zn,Cu,Mg,Al,Fe,P,K,Si,Se,Ba,Mn,M015种元素含量,并对各元素进行了加标回收实验,黑豆和红小豆中各元素的平均回收率在93.11%~102.15%,相对标准偏(RSD)在0.83%0~2.8%,检出限介于0.11~14.09Fg/L。建立了简便、快速、准确和稳定的测定黑豆和红小豆中元素的测定方法。结果显示在黑豆和红小豆中K,Ca,P,Mg,Mn,Fe,Zn等常量元素和微量元素含量较高。红小豆中Ca,Mg,Fe,Zn等营养元素的含量较黑豆中的高。 相似文献
5.
ICP-AES法测定锡铅焊料中铜铁镉锌铝铋 总被引:4,自引:0,他引:4
锡铅焊料试样经盐酸、硝酸分解后,加入一定量的硫酸沉淀分离基体铅,以盐酸一氢溴酸排锡后,采用ICP—AES法同时测定铜、铁、镉、锌、铝、铋。方法没有谱线和背景干扰,检出限铜为0.000034%,铁为0.000038%,镉为0.000026%,锌为0.000071%,铝为0.00025%,铋为0.00060%,回收率在91.09/5~99.2%之间。完全满足锡铅焊料中的铜、铁、镉、锌、铝、铋测定的要求。 相似文献
6.
采用等离子发射光谱法同时测定碳化硼颗粒增强铝基复合材料中Al,Si,B,Mg,Cu,Fe等元素的含量。分析了各元素之间以及基体的光谱谱线相互干扰情况,对标准溶液采取与样品大致相同的基体匹配方式,消除了基体干扰,使测定结果更加准确。 相似文献
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研究了小功率空气-氩气混合气冷却ICP中4种元素(钙、钡、铜、锌)、8和谱线的强度和信背比随冷却气组成及观测高工估算了折中条件下的检出限。对于离子线及激发电位较高的原子线,冷却气中引入体积分数为5-10%空气后,谱线强度最大并大于Ar-ICP中数值;对于激发发电位较低的原子线,随着气中空气含量的增大其谱线强度逐渐减小,谱线的信背比则与激发电位及谱线波长有关。 相似文献
11.
Evaluation of inductively coupled plasma optical emission spectrometers with axially and radially viewed configurations 总被引:2,自引:0,他引:2
Fernando V Silva Lilian C Trevizan Cntia S Silva Ana Rita A Nogueira Joaquim A Nbrega 《Spectrochimica Acta Part B: Atomic Spectroscopy》2002,57(12):335-1913
The analytical performance of two inductively coupled plasma optical emission spectrometers with axially and radially viewed configurations, equipped with charge coupled device solid-state detectors was evaluated using Ar, Ba, Mg, and Ni as test elements. Both instruments have similar Echelle optical arrangements and radio-frequency generators, differing only in the viewing mode and in the diameter of the central injector tube, i.e. 2.3 for the axially and 1.4 mm for the radially viewed ICP. The figures of merit evaluated were: warm-up time, short- and long-term stabilities, UV and VIS spectral resolution and limit of detection (LOD) for Ni in 0.14 mol l−1 HNO3 and 1000 mg l−1 Cr media, respectively. The influence of residual carbon content on background equivalent concentration (BEC) and sensitivity attained for Al, As, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Se and Zn was also investigated in both viewing modes. The robustness, short- and long-term stabilities, and UV and VIS spectral resolutions were similar for both configurations. For the radially viewed equipment, the warm-up time was at least a factor of 2 shorter than that for the axially viewed configuration. On the other hand, the sensitivity attained for Ni with the axially viewed arrangement was approximately 20 times better than that with the radially viewed. In both viewing modes, and for most of the evaluated elements, the values of BEC and LOD were similar for all studied carbon concentrations (from 10 to 10 000 mg l−1 C) when working with robust plasma conditions. The Mg II/Mg I ratio at an applied power of 1.3 kW and a nebulizer gas flow-rate of 0.90 and 0.70 l min−1 for axially and radially viewed configurations were 10.6 and 13.7, respectively. Quantitative determinations were successfully performed using both systems. 相似文献
12.
The linear relationship between Ca and Na interferences and energy potentials for a wide range of atomic and ionic lines is used to compensate for variable intensity suppression in robust axially and radially viewed inductively coupled plasmas (ICPs). In the axial configuration, intensity attenuation varied from 0 to 40% in the presence of 0.5% Ca and Na. In the radially viewed ICP, interferences were smaller, varying from 5 to 15% for 0.5% Na and from 10 to 30% for 0.5% Ca. Signal attenuation was broadly a linear function of the energies of the spectral lines. These linear functions were estimated by using spectral lines covering the energy range from Sb I 206.833 (5.98 eV), Y II 371.209 and Sc II 361.384 (9.9 eV), Sc II 255.237 (11.42 eV), and Be II 313.042 (13.28 eV) nm. These functions were then used as variable internal standards to compensate for Ca, Na, and mixed Ca–Na matrix effects. Whereas analyte recoveries without compensation varied from about 40 to 90%, they varied mostly from 100 ± 5% when these functions were used. In the presence of Ca and Na, the Mg II 280.270/Mg I 285.213 nm intensity ratio decreased from about 12 for an aqueous solution to 9 at 1.5 kW. Such values confirm that the radially and axially viewed ICPs were robust. 相似文献
13.
乙醇对低功率ICP光源的影响 总被引:1,自引:0,他引:1
研究了在低功率他激高频发生器条件下,乙醇对ICP-AES的影响。乙醇引入试液后导致粘度增加,表面张力、密度下降,试样提升量降低,等离子体激发温度和气体温度下降,Ca,Mg,Ni,Cu,Pb等常见元素灵敏度降低而稀土元素的灵敏度得到改善。讨论了乙醇对低功率ICP光源的影响。 相似文献
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《Spectrochimica Acta Part B: Atomic Spectroscopy》2004,59(1):41-58
A novel optical configuration for inductively coupled plasma (ICP)-atomic emission spectrometry is presented. Plasma emission is measured axially via the bottom end of the ICP torch. Analytical performance, such as increase in signal-to-background ratio (SBR) over radially viewed ICP and linear dynamic range, is comparable to that of end-on axially viewed ICP reported in the literatures. Under typical ICP operating conditions (forward power=1.0–1.6 kW, central channel gas flow rate=0.8–1.4 l/min), SBR is generally five times or more that of radial-viewing mode (observation heights=3–20 mm) for atomic lines of elements of low to medium ionization potential (Na, K, Sr and Ba). The enhancement factor in SBR is two to four times for ionic lines (e.g. MgII) and atomic lines of elements of high ionization potential (Zn). The influence of ICP forward power and carrier gas flow rate on analyte emission intensity and SBR were also studied. Similar to radially viewed ICP, as forward power increases, the net emission intensity increases and SBR decreases. Using a constant flux of analyte aerosols, the net intensity decreases as the central channel gas flow rate increases. No trend of SBR vs. central channel gas flow rate, however, is found. The linear dynamic range starts and ends at analyte concentration 0.5–1 order of magnitude lower than the corresponding radial-viewing mode. As a result, the span of linear dynamic range is similar for all viewing modes. Matrix effects of K and Ca on atomic lines are different from those reported for end-on axially viewed ICPs, probably due to the difference in the plasma regions that were probed. The matrix effects on ionic lines, however, are similar in magnitude. 相似文献
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The effects and benefits of N2 addition to the central channel of the ICP through the nebulizer gas used in ICP OES with axial view configuration were investigated in the present study. The N2 flow rate, nebulizer gas flow rate, RF power and sample uptake rate were evaluated and compared for two sample introduction systems (pneumatic nebulization/aerosol desolvation and conventional pneumatic nebulization). It was observed that N2 did not affect solution nebulization and aerosol transport but affects the ICP characteristics. The higher thermal conductivity of N2 (in comparison with Ar) changes energy distribution in the ICP, observed by monitoring the signals of Ar emission lines and sodium emission. The ratio Mg(II)-280.270 nm/Mg(I)-285.213 nm was utilized as a diagnostic tool for plasma robustness. The addition of N2 (20 mL min−1) increased plasma robustness significantly and mitigated effects caused by Na, K and Ca. For 40 spectral lines evaluated, it was observed that the emission signals of ionic spectral lines were in general more affected by N2 than those of atomic spectral lines. Detection limits, precision, sensitivity and linearity of calibration curves obtained using N2-Ar-ICP were almost similar to those obtained using Ar-ICP. The analysis of 5 different reference materials revealed that accuracy was not degraded by adding N2 to the Ar-ICP. 相似文献
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M. Iglsias T. Vaculovic J. Studynkova E. Poussel J.M. Mermet 《Spectrochimica Acta Part B: Atomic Spectroscopy》2004,59(12):1841-1850
In order to study in ICP-AES, the influence of the plasma operating conditions, power and carrier gas flow rate, and of the optical transition on non-spectral matrix interferences, line-rich elements such as Mn, Cr and Cu have been selected. Selection of a large pool of lines was possible because of the use of multichannel solid-state detection. An axially viewed plasma was used. Matrices were K, Na, Li, Ca and Mg. Matrix effect was evaluated by comparing the signals for test elements in water. Use of robust conditions led to an almost flat response, while non-robust conditions led to a significant scattering of the signal changes. In the case of Mn, the z7P Mn multiplet was exemplified as it contains not only the most Mn sensitive line, the Mn II 257.610 nm resonance line, but also the 259.372 and 260.568 nm resonance lines, and the non-resonant Mn II 343.897 nm line. Even under robust conditions, the non-resonant line exhibited a different behavior. The difference with the other resonance lines was reduced by using an axially viewed ICP with a large injector id, or suppressed by using a radially viewed ICP. In the case of Cr, the z6D Cr II multiplet was selected as it contains three resonant lines linked to the a6S fundamental, and other non-resonant lines. The behavior was identical under robust conditions, while an abnormal behavior was observed for the Cr II 334.78 nm line under non-robust conditions, depending on the extent of these non-robust conditions. Cu was an interesting element as ionic lines lie in the energy sum range 15.96–16.26 eV, i.e. slightly above the Ar ionization energy. It was shown that, under robust conditions, the line behavior was not similar although the energy range was small. Moreover, this behavior was depending on the ICP system used for the experiment. It was concluded that not only the magnitude of matrix effects depends on the operating conditions but also may depend on the optical transition, illustrating the complexity of these effects. 相似文献
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Julio C. J. Silva Daniele M. Santos Solange Cadore Joaquim A. Nobrega Nivaldo Baccan 《Microchemical Journal》2004,77(2):185-190
In this investigation, samples of whole bovine milk were diluted with water-soluble tertiary amines solution and introduced in two axially viewed inductively coupled plasma optical emission spectrometer (ICP OES) instruments equipped with different interfaces (shear gas and end-on gas interface). The accuracy and the Mg II (280.2 nm)/Mg I (285.2 nm) ratio were evaluated. Higher values for Mg II/Mg I were observed with the shear gas interface. However, these values were less affected by changes of instrumental parameters when using the end-on gas interface. Results with suitable accuracy were obtained for a certified reference material of powdered whole milk (NIST SRM 8435) using instruments equipped with each interface. 相似文献
18.
《Spectrochimica Acta Part B: Atomic Spectroscopy》2001,56(4):409-418
The torch wall is cooled largely by air passing through a cooling jacket added to the outside of a Fassel torch. The plasma is viewed axially through a cooled cone interface centered on the axial channel. The outer argon gas flow can be reduced to 7 l min−1 with no compromise in performance or torch lifetime. The plasma exhibits the same ‘robustness index’ and interference effects from Na as the conventional, high-flow ICP supplied with the particular spectrometer used. Detection limits (DL) for lines at ∼200 nm are poorer by approximately a factor of two, while those for lines at ∼400 nm are actually better than values typically seen for the same lines by axial viewing of a conventional, high-flow ICP. 相似文献
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The method of ultrasound-assisted extraction followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of trace element concentrations (arsenic, copper, lead, antimony, and zinc) in shooting range areas was optimized. Optimization was achieved not only on the basis of the analysis of appropriate standard reference materials but also on that of 31 synthetic mixtures of matrix and analyte elements (aluminum, antimony, arsenic, calcium, copper, lead, iron, manganese, silicon, and zinc), in five concentrations. All the measurements were performed in robust plasma conditions which were tested by measuring the Mg II 280.270 nm/Mg I 285.213 nm line intensity ratio. The highest Mg II 280.270 nm/Mg I 285.213 nm line intensity ratios were observed when a nebulizer gas flow of 0.8 L min−1, auxiliary gas flow of 0.2 L min−1 and plasma power of 1400 W were used for both the axially and radially viewed plasmas. The analysis of 31 synthetic mixtures of the selected elements showed that As concentrations could be accurately determined with axially viewed plasma alone. The determination of Pb and Sb could be performed with either axially or radially viewed plasma whereas, surprisingly, Cu could be determined with high accuracy using radial plasma alone with a power of 1400 W. All the elements investigated were determined with high accuracy using robust plasma conditions and a combination of axially and radially viewed plasmas. The total recoveries of elements from SRM 2710 (Montana soil) and SRM 2782 (Industrial sludge) were highly comparable to leach recoveries certified by the National Institute of Standards and Technology (NIST). 相似文献