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Evaluation of two atomisation modes for direct determination of molybdenum in complex matrices by ultrasonic slurry sampling-electrothermal atomic absorption spectrometry

机译:超声浆液采样-电热原子吸收光谱法直接测定复杂基质中钼的两种雾化模式的评估

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摘要

Tube wall (TWA) and L'vov platform (LPA) atomisations were compared for the direct determination of molybdenum (Mo) in coal fly ash by slurry sampling-electrothermal atomic absorption spectrometry (ETAAS).For both atomisation modes eight chemical modifiers were tested,namely HNO_3,Pd(NO_3))2,Mg(NO_3)_2,Pd + Mg(NO_3)_2,reduced Pd,BaF_2,Ir and HF.The interfering effects of major and minor concomitants of samples on Mo signals and memory effects were also evaluated.BaF2 and Pd(NO_3)_2 + Mg(NO_3)_2 mixture were selected for TWA and LPA,respectively.Standard addition calibration is needed in both cases.The best peak performance,memory effect reduction,within-run precision (6% versus 9% R.S.D.),and sensitivity (m_a = 7.5 pg versus 15.2pg) were achieved with TWA compared to LPA.Both atomisation modes gave good analytical recoveries (94-102%),but the analysis of a certified coal fly ash (NIST SRM 1633a) only was accurate using TWA.Additionally,the urban dust NIST SRM 1629a was analysed.
机译:比较了管壁(TWA)和L'vov平台(LPA)的雾化率,通过浆液采样-电热原子吸收光谱法(ETAAS)直接测定粉煤灰中的钼(Mo)。对于两种雾化模式,均测试了八种化学改性剂,即HNO_3,Pd(NO_3))2,Mg(NO_3)_2,Pd + Mg(NO_3)_2,降低了Pd,BaF_2,Ir和HF。样品的主要和次要伴随物对Mo信号的干扰作用和记忆效应TWA和LPA分别选择了BaF2和Pd(NO_3)_2 + Mg(NO_3)_2混合物。两种情况都需要标准加标定。最佳峰性能,记忆效应降低,运行内精密度(与LPA相比,TWA达到了6%的RSD(相对于9%的RSD)和灵敏度(m_a = 7.5 pg对15.2 pg)。两种雾化模式均具有良好的分析回收率(94-102%),但经过认证的粉煤灰分析(NIST SRM 1633a)仅在使用TWA时才是准确的。此外,还分析了城市灰尘NIST SRM 1629a。

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