Determination of Pd,Rh, Pt,Au in road dust by electrothermal vaporization inductively coupled plasma mass spectrometry with slurry sampling

Inductively coupled plasma mass spectrometry coupled with ultrasonic slurry sampling electrothermal vaporization (USS-ETV-ICP-MS) has been applied to determine Pd, Rh, Pt and Au in 0.5% m/v slurries of several road dust samples. 2% m/v ammonium pyrrolidine dithiocarbamate (APDC) was used as the modifier to enhance the ion count. The influence of instrument operating conditions, slurry preparation and interferences on the ion count was reported. This method has been applied to the determination of Pd, Rh, Pt and Au in BCR 723 Road Dust and NIST SRM 2709 San Joaquin Soil reference materials and two road dust samples collected locally. The analysis results of the standard reference materials agreed with the certified values. Precision between sample replicates was better than 10% for all the determinations. The method detection limits estimated from standard addition curves were 0.9, 0.4, 0.6 and 0.4 ng g⁻¹ for Pd, Rh, Pt and Au, respectively, in original dust samples.     

Determination of arsenic in mussels by slurry sampling and electrothermal atomic absorption spectrometry (ETAAS)

A method for the determination of arsenic in slurries of mussel tissue using palladium-magnesium nitrate as modifier was optimized. The slurry was stabilized by a 0.015% (v/v) of Triton X-100. To achieve complete mineralization the slurries were ashed at 480 °C for 10s in an air flow (50 ml/min) and at 1200 °C for 15s in an argon flow (300 ml/min) in the presence of Pd—Mg(NO₃)₂ as modifier. The optimum atomization temperature was 2200 °C. The precision and accuracy of the method were studied using the Reference Material BCR n ° 278 Mussel Tissue (Mytilus edulis). The detection limit (LOD) of the final slurry solution was 1 g/l of arsenic corresponding to an arsenic level in the mussel of 1.3 g/g, for a 0.5% (m/v) slurry. Results of calibration using aqueous standards and the standard additions method were compared. The method was applied to the determination of arsenic in mussels from the Galician coast. The levels found lie between 2 and 9.3 g/g of arsenic.     

A Simple and Fast Method for Manganese Determination in Antihypertensive Drugs by Slurry Sampling Graphite Furnace Atomic Absorption Spectrometry

Abstract

A simple and rapid procedure for the determination of manganese in anti‐hypertensive drugs is proposed. The samples were treated with dilute nitric acid (1.2% v/v) with stirring using a vortex stirrer to yield a slurry. To determine the best conditions for analysis by graphite furnace atomic absorption spectrometry (GF AAS), a planning factorial was initially employed that demonstrated that the non‐use of chemical modifiers and the use of lower pyrolysis temperatures were more appropriate. Next, the pyrolysis and atomization temperature curves were obtained. The best pyrolysis and atomization temperatures encountered were 500 and 2200°C, respectively. Calibration was performed by matrix matching. The characteristic mass was 0.70±0.14 pg (the recommended mass was 0.60 pg); the limits of detection and quantification were 0.23 and 0.77 µg l^?1, respectively. The precision obtained in the intra‐ and inter‐assay studies of the drug spiked with 0.5, 1.0 and 1.5 µg l^?1 of Mn did not exceed 11% (n=7). Recovery studies of the drug spiked with three levels (n=7) of Mn yielded results between 101.0±4.5 and 116.3±9.7%. The results of an analysis of a certified urine sample (two levels of Mn) agreed at a 95% level of confidence. Forty‐eight antihypertensive drug samples were analyzed, and the results varied from 2.9 ng to 1.9 µg of Mn per capsule^?1.     

醋酸甲羟孕酮与β-环糊精包络作用的光谱研究及应用

用紫外吸收、荧光光谱法对水溶液中β－环糊精（β－ＣＤ）与醋酸甲羟孕酮（ＭＡ）主客体包络物的光谱行为进行了研究．利用改进的Ｂｅｎｅｓｉ－Ｈｉｌｄｅｂｒａｎｄ法测定了包络物的形成常数，初步探讨了某些水溶性一元醇的引入对该包络物形成及荧光性质的影响，并提出了测定ＭＡ的高灵敏度荧光光度新方法，方法的最低检出限为８．９×１０－９ｍｏｌ·Ｌ－１．用该法测定样品中ＭＡ的结果令人满意，回收率为９７．９％～１０１．７％，平均回收率为９９．９％（ｎ＝５）     

Determination of lead in environmental reference materials (plant materials) by slurry-ETA-AAS

Slurry-ETA-AAS is used to determine lead in plant materials. The stability of the slurry was studied and it was shown that, when NH₄H₂PO₄ modifier is added, the shape of the time resolved absorbance signal for the sample and the standards is similar and the calibration line obtained using aqueous standards is parallel to the standard addition line. Results obtained for several reference materials (lead contents between 6.1 and 64.4 g/g) were in good agreement with the certified value, the relative standard deviation being 3–9%.     

硅片研磨表面状态的改善和研磨液的改进

在硅片研磨过程中,由于应力的积累和剧烈的机械作用,硅片表面损伤严重,碎片率增加.介绍了一种改进的研磨液,不但把剧烈的机械作用转变为比较缓和的化学-机械作用,还能起到其他较好的辅助作用并对其各成分作用,进行了理论分析.硅片表面状态得到了一定程度的改善,提高了生产效率.     

ULSI中多层Cu布线CMP表面粗糙度的分析和研究

分析介绍了Cu层表面粗糙度对器件性能的影响以及超大规模集成电路中多层Cu布线CMP的作用机理,研究分析了碱性抛光液对Cu的表面粗糙度的影响因素,如磨料、氧化剂、pH值、表面活性剂等对表面粗糙度的影响。实验证明,在一定的抛光条件下,选用SiO2为磨料、双氧水为氧化剂的碱性抛光液可以有效降低Cu层的表面粗糙度,使之达到纳米级,得到良好的抛光效果,从而解决了超大规模集成电路多层Cu布线化学机械抛光中比较重要的技术问题。     

铜互连制程中酸碱性抛光液的平坦化效果评估

We observed and analyzed the acid and HEBUT alkaline of Cu chemical mechanical polishing(CMP)slurry to evaluate their effects. Material analysis has shown that the planarity surfaces and the removal rate of alkaline slurry are better than the acid slurry during metal CMP processes. The global surface roughness and the small-scale surface roughness by 1010 m2 of copper film polished by the SVTC slurry are 1.127 nm and2.49 nm. However, it is found that the surface roughnesses of copper films polished by the HEBUT slurry are 0.728 nm and 0.215 nm. All other things being equal, the remaining step heights of copper films polished by the SVTC slurry and HEBUT slurry are respectively 150 nm and 50 nm. At the end of the polishing process, the dishing heights of the HEBUT slurry and the SVTC slurry are approximately both 30 nm, the erosion heights of the HEBUT slurry and the SVTC slurry are approximately both 20 nm. The surface states of the copper film after CMP are tested,and the AFM results of two samples are obviously seen. The surface polished by SVTC slurry shows many spikes.This indicates that the HEBUT alkaline slurry is promising for inter-level dielectric(ILD) applications in ultra large-scale integrated circuits(ULSI) technology.     

油浆高温快速裂解过程的气固相产物研究

采用高频炉快速热解装置研究油浆的高温快速热解特性,考察了热解温度、氮气流量对气固相产物的组成和产率的影响。温度是影响气相产物产率的关键因素,气相产物主要为甲烷、氢气和乙烯,升高温度可提高甲烷和氢气的产率,而乙烯产率受高温下二次反应的影响在800℃到达最大值后逐渐降低,乙烷、丙烯产率较小且受二次反应的影响在700℃到达最大值后逐渐降低,温度高于800℃时会有少量乙炔生成且升温可提高乙炔产率。增加氮气流量可降低甲烷、氢气分压,缩短乙烯、丙烯等在高温区的停留时间,从而增加气相产物的产率。积炭产率随热解温度升高迅速增加,氮气流量的增加能够削弱二次反应从而降低积炭产率。