端视ICP-AES系统分析性能研究──Ⅰ．在稀土分析中的应用

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。     

端视ICP-AES法测定钕铁硼永磁材料中常量及微量元素

报道了用高灵敏度的电感耦合等离子体原子发射光谱法（ＩＣＰ－ＡＥＳ）直接测定钕铁硼永磁材料中常量、少量及微量元素：Ｎｄ、Ｆｅ、Ｃｏ、Ｂ、Ｌａ、Ｃｅ、Ｐｒ、Ｄｙ、Ｇｄ、Ｓｍ、Ａｌ、Ｍｎ、Ｃａ、Ｍｇ、Ｇａ和Ｓｉ的分析方法。选择了合适的分析线，研究了基体元素Ｎｄ、Ｆｅ、Ｃｏ对被测杂质元素分析线的光谱干扰，采用基体匹配与背景扣除法进行校正。各被测元素的检出限为０．５～３０μｇ／Ｌ，回收率为９２～１１０％，相对标准偏差小于７％。本法已用于钕铁硼产品的快速检验，并获得了满意的结果。     

端视ICP－AES系统分析性能研究──Ⅰ．在稀土分析中的应用

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。     

微波消解-端视ICP-AES测定茶叶中微量重金属元素

采用微波消解-端视等离子体原子发射光谱(ICP-AES)测定茶叶中微量重金属元素Pb、As、Cd、Cu、Fe,并对ICP-AES工作参数及条件进行了优化和选择。Pb、As、Cd、Cu、Fe的检出限分别为2.9×10-3μg/mL、5.2×10-3μg/mL、0.056×10-3μg/mL、0.55×10-3μg/mL、0.59×10-3μg/mL,线性范围为0~10000μg/L,相对标准偏差为1.7%~8.5%;回收率为90%~104%。该方法与国标法比较,结果无显著性差异。本法能用于茶叶测定。     

端视ICP-AES法同时测定玩具涂料中可溶性铅、镉、汞、砷、铬、锑、硒和钡

采用端视电感耦合等离子体原子发射光谱(ICP-AES)法同时测定玩具涂料中可溶性铅、镉、汞、砷、铬、锑、硒和钡.对仪器的工作参数和被测元素的分析谱线进行了优化和选择.铅、镉、汞、砷、铬、锑、硒和钡的检出限分别为0.006、0.0009、0.012、0.023、0.000 8、0.013、0.030和0.0006 mg/L.定量下限分别为0.99、0.15、2.0、3.8、0.14、2.2、5.0和0.10 mg/kg.相对标准偏差为0.76%～2.72%(n=8),加标回收率为96.0%～104.0%.该法适用于玩具涂料中铅、镉、汞、砷、铬、锑、硒和钡的快速测定.     

ICP—AES中内标法的应用研究：Ⅲ.用内标法校正基体干扰

通过观测基体对分析元素发射强度的干扰情况，分析了扰机制，从而确定用来正基体干扰的内村元素与分析元素的匹配条件。实验结果表明，只要选择合适的内标元素，可以校正基体干扰。     

电感耦合等离子体发射光谱分析中基体干扰校正方法的研究

本文提出一种校正ICP-AES基体干扰的新方法——样品标准加入法,并以4个标准参考物质进行验证,证明该方法结果可靠。     

ICP－AES中内标法的应用研究 Ⅲ．用内标法校正基体干扰

通过观测基体对分析元素发射强度的干扰情况,分析干扰机制,从而确定用来校正基体干扰的内标元素与分析元素的匹配条件。实验结果表明,只要选择合适的内标元素,可以校正基体干扰。     

ICP－AES法检测Sr、Ca、Mg、P在海带多糖中的分布

应用ＩＣＰ－ＡＥＳ技术，检测了Ｓｒ、Ｃａ、Ｍｇ、Ｐ在海带叶状体的褐藻淀粉、藻酸盐、褐藻糖胶和纤维素等多糖中的分布，发现锶主要存在于褐藻糖胶中［９．６×１０－３（糖干重），占叶状体总锶的４７．２％］，而其他成分中的锶含量都较低。提示锶与维持藻体结构有关。     

ICP-AES中Ca、Al之间相互干扰的研究

本文在不同条件下比较详细地研究了Ca与Al在ICP-AES中的相互干扰,结果表明:这种干扰的垂直空间分布与其它元素的基体效应不同,特别在低观察区域Ca、Al之间呈现较为明显的相互抑制效应,说明Ca和Al之间产生了溶质挥发干扰。对分析条件特别是入射功率、载气流量及观察高度进行最优化可以使这种干扰减至最小。     

电荷注入检测器—端视等离子体原子发射光谱中分析动态范围

实验研究了电荷注入检测器－端视电感耦合等离子体光谱中分析动态范围，测量了ＡＬ，Ｂ、Ｂｅ，Ｃｄ，Ｃｕ，Ｃｏ，Ｆｅ，Ｌｉ，Ｓｒ，Ｖ，Ｋ，Ｓｒ等１２个元素的不同光谱级次的４４条分析工作曲线。结果表明，分析范围为４－５个数量级，无明显自吸收，Ｌｏｍａｋｉｎ公式的自吸收系数ｂ＝１，说明在ＣＩＤ－ＡＶＩＣＰ光谱中有较宽的分析动态范围 。     

On Atomization of Calcium,Magnesium and Antimony from ThO2 Matrix by Atomic Absorption Spectrometric Techniques

ABSTRACT

Atomic Absorption Spectrometric methods (AAS) developed for the direct determination of Ca and Mg using flame-AAS technique have linear ranges of 0.1-2.0 μg/ml and 0.025-0.4 μg/ml with thorium concentrations optimized at 2.5 and 0.5 mg/ml, respectively, while the analytical range obtained for Sb using electrothermal-AAS technique is 0.002-0.1 μg/ml with Th sample aliquot of 2.5 mg/ml. The precision of determinations for both the techniques as evaluated from analyses of synthetic samples is 5% RSD or better. Probable mechanism for atom formation for Sb has been discussed in detail. In addition, role of chemical modifiers in enhancing the analyte signal has also been discussed.     

大功率微波诱导空气等离子体发射光谱中易电离元素的基体干扰研究

研究了由Okamoto腔产生的大功率微波诱导空气等离子体发射光谱中易电离元素Na和Ca的基体干扰。结果表明,Na和Ca的存在可使电离能较低的元素的原子线的发射强度增强,而使电离能较高的元素的原子线和几乎所有的离子线的发射强度降低。基体干扰随Na和Ca浓度的增大而增强,随等离子体微波功率的增大而减弱。Na和Ca的存在致使等离子体激发温度降低,电子密度增大。基体干扰是由于易电离元素使待测元素在等离子体中的电离平衡移动和激发能力减弱所致。     

Advantages and effects of nitrogen doping into the central channel of plasma in axially viewed-inductively coupled plasma optical emission spectrometry

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.     

Study of Matrix Effects on Determination of Trace Elements in Aluminum,Using Inductively Coupled Plasma Atomic Emission Spectrometry, 1) Selection of Spectral Lines.

Abstract

The effect of an aluminum matrix on the determination of B, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Ni, Si and Zn was studied. These elements are expected to be present in high purity Al base materials. 45 spectral lines of these elements were scanned in a spectral window of 60 pm. Background equivalent concentrations were calculated and compared with existing data. Interference free spectral lines, one for each element, have been recommended to be used for analysis. Depression effects due to the Al matrix were calculated at the selected lines.     

Rotational temperatures and LTE in argon ICP

Rotational temperatures deduced from OH molecular spectra have been studied in an analytical argon inductively coupled plasma for various operating conditions. The Boltzmann plots are often curved and temperatures are very different from those deduced from atomic Boltzmann plots or from other molecular species like N₂. Generally non-equilibrium is deduced from these observations. But thermal stability of OH and local gradient in the droplet surroundings can to a great part explain these phenomena. Complex simulations seem useful for a satisfactory explanation.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria     

光谱复杂的稀土基体中稀土杂质ICP光谱测定的一些问题

ICP激发光源以其独特的功能使ICP/AES技术在稀土分析中的应用日益广泛,在一定程度上取代了经典的直流电弧光谱法,但应指出,由于常规雾化器的低雾化效率(≤5％)和试样的高倍稀释,ICP/AES技术的实际检测能力的改善并不明显,本文用ICP光谱法测定了     

ICP－AES法同时测定高纯碳酸钡中锶钙镁铁

用ＩＣＰＡＥＳ法同时测定高纯碳酸钡中锶、钙、镁、铁考察了谱线选择、基体的影响，确定了仪器最优化工作参数方法回收率为９６—１０７％，ＲＳＤ为４７１－９．６２％