双铂网雾化和超声雾化进样系统对ICP-AES分析性能的影响

从元素检出限、基体效应、ICP稳健性及记忆效应方面实验研究了双铂网雾化与超声雾化两种进样方式对ICP-AES分析性能的影响。结果表明,在超声雾化进样条件下,Cu,Pb,Zn,Cr,Cd,Ni的检出限较双铂网雾化的检出限降低了6～23倍;在基体效应方面,超声雾化进样时基体对元素原子及离子谱线强度的影响均较双铂网雾化系统明显,元素谱线增强/减弱的幅度受元素谱线、基体组成和浓度的影响;Ca和Mg基体对谱线强度的影响强于K和Na基体;离子谱线受基体的影响明显强于原子谱线。超声雾化系统进样时ICP的稳健性要劣于双铂网雾化系统,而且超声雾化系统的记忆效应较双铂网雾化器严重。     

电热蒸发等离子体发射光谱的研究

等离子体发射光谱技术已迅速成为一种常规的分析工具,但是进样方式仍然是目前继续研究的重要课题。液体进样常用气动雾化,超声雾化、电热蒸发和氢化物发生等手段把样品引入ICP;固体进样是把固体样品直接或者气化后引入ICP。相比之下,液体进样,特别是气动雾化法仍是目前较理想的方法。电热蒸发法用作ICP的进样已由一些分     

流动注射-ICP-AES多元素同时分析及NaCl基体干扰效应的研究

本文研究了以流动注射进样的ICP-AES分析方法和NaCl的基体效应。0.25-2.5%NaCl对11个元素的影响结果表明,FI进样可克服常规连续雾化的信号漂移,从而改善了测量精度。不同功率下的NaCl基体的影响不同。结果表明,NaCl的基体效应主要存在于气溶胶微粒在ICP中的蒸发—原子化—激发过程。     

超声雾化空气—氩ICP—AES的检出限

医用超声雾化强器改装后的ＩＣＰ－ＡＥＳ进样装置，在高频功率３．８×０．８０ｋＷ载气流量０．８０Ｌ．ｍｉｎ＾－１，观察高度１．０ｃｍ的折衷条件下，测定了２８种元素的检出限，１５种稀土元素中Ｄｙ，Ｅｕ，Ｈｏ，Ｙ和Ｙｂ的检出限低于１μｇ．Ｌ＾－１。     

流动注射-电感耦合等离子体发射光谱法测定天然水中的钙和镁

本文采用流动注射－电感耦合等离子体发现光谱联用技术测定了天然水中的钙、镁元素。考察了试液的雾化和曝光时间及载气压力等因素对分析信号的影响。通过与气动连续进样的对比，测出了钙、镁在流动注射进样下的分散系数。本法在测定钙、镁含量高的水性时，不需对试样进行稀释处理。对五个水样中钙、镁的分析结果与EDTA络合滴定法相吻合。     

MPT-AES测定奶粉中的微量金属元素

用微波等离子体(MPT)为激发光源,氩气为等离子体工作气体,用气动雾化进样,以校准曲线法研究了微波等离子体炬原子发射光谱法(MPT-AES)测定奶粉中的镁、钠。详细考察了溶液中盐酸浓度、硝酸浓度、共存离子浓度、微波前向功率、载气流量、工作气流量等实验参数对测定的影响。测定结果表明,镁和钠质量浓度的检出限分别为0.36、0.75μg/L,RSD(n=6)≤0.41%,线性范围分别为0.02—9mg/L、0.02—4mg/L,MPT-AES提高了测定奶粉中微量金属元素含量的速度和准确度。     

电感耦合等离子体-原子发射光谱法测定松口蘑中的铝

用不同的消解方式处理试样松口蘑(SKM 20080604),电感耦合等离子体-原子发射光谱法(ICP-AES)测定松口蘑中铝含量。该方法具有灵敏度高、检出限低、精密度好、效率高等优点,其检出限为0.18mg·mL-1,RSD为1.96%。若使用超声雾化器雾化装置,检出限为0.05mg·mL-1,RSD为5.49%。采用硫酸消解方式,能够明显提高松口蘑的消解效率;样品的酸度过高会影响测定结果,样品中硫酸含量低于2.5%以下时,可得到满意的结果。同时,可用该分析方法测定美味牛肝菌、大白口蘑中的铝。     

悬浮液雾化进样感耦等离子体基本参数研究——Ⅱ等离子体电子密度测定

研究了悬浮液雾化进样感耦等离子体原子发射光谱基本参数-等离子体电子密度的测定。实验使用Stark效应常用的谱线H_β线来计算等离子体电子密度。测定结果表明悬浮液雾化进样同水溶液雾化进样感耦等离子体原子发射光谱时等离子体电子密度没有发生显著的变化,数值基本上为1015数量级。固含量高达10％ TiO₂悬浮液雾化进样等离子体原子发射光谱,电子密度测定结果仅有微小的降低。高固含量悬浮液雾化进样等离子体原子发射光谱没有显著地影响等离子体电子密度,有助于使用高固含量悬浮液雾化进样等离子体原子发射光谱来进行痕量元素分析测定。     

超声平衡雾化集中进样火焰原子吸收法的研究

本文提出了一种采用新进样方式的超声雾化火焰原子吸收法。该法对Cu、Ag、Pb、Cd等元素的特征浓度较一般气动雾化进样火焰原子吸收法有近一个数量级的改善。若与石英缝管技术配合使用,则对Cu、Ag、Pb、Cd的特征浓度分别为2.0、1.4、8.0、0.54ppb。实验证明,方法的精密度和准确度都令人满意。     

气相色谱和原子荧光联用测定生物和沉积物样品中甲基汞

提出了一种气相色谱和原子荧光在线联用测定甲基汞的方法。对气相色谱和原子荧光的在线联用进行了设计,优化了进样口温度、载气流速、尾吹气流量及氩气流量等实验条件。在最佳仪器条件下,甲基汞(MMC)和乙基汞(EMC)的绝对检出限(3σ)可达0.005 ng。对于10 ng·mL-1 MMC和EMC标准溶液,连续5次进样测得精密度(RSD)分别为2.5％和1.3％。对标准参考物(DORM-2)的分析结果与标准值一致。两个沉积物中甲基汞的加标回收率分别为70％和77％。方法准确、灵敏,可应用于生物和沉积物样品中甲基汞的分析。     

菲涅尔透镜聚焦声泳打印装置设计及实验研究*

针对现有的喷墨打印技术需根据喷印材料的特性定制而较难直接用于不同材料打印的问题,设计了一种基于菲涅尔透镜聚焦的声泳打印装置,该装置由超声发生器、超声换能器、菲涅尔透镜以及供液系统组成。首先,利用COMSOL软件模拟液滴在声辐射力作用下的滴落过程,并分析了超声发生器功率、喷嘴到基底距离、菲涅尔透镜厚度等参数对声场压力分布的影响,以及声场压力、喷嘴直径及材料粘度对液滴喷射过程的影响。其次,采用构建的声泳打印装置进行喷射成滴实验,通过调整超声发生器输出功率实现了不同粘度的聚乙二醇溶液的喷射以及UV胶的喷射。实验结果表明：该微滴喷射系统能产生一致性较好的微滴,喷印出的微透镜尺寸波动范围在2%以内,证明了该装置的稳定性以及实现了不同材料微滴喷射的可行性。     

Method Development for Simultaneous Determination of Transition (Au,Ag, Cd,Cu, Mn,Ni, Pb,Zn) and Noble (Pd,Pt, Rh) Metal Volatile Species by Microwave-Induced Plasma Spectrometry Using Ultrasonic Micronebulizer Dual Capillary Sample Introduction System

ABSTRACT

The commercial ultrasonic nebulizer NOVA-DUO (Optolab, Warsaw, Poland) has been evaluated for the simultaneous determination of transition (Au, Ag, Cd, Cu, Mn, Ni, Pb, Zn) and noble (Pd, Pt, Rh) volatile metal species by microwave induced plasma–optical emission spectrometry (MIP-OES). Simultaneous mixing and nebulization of the two solutions (acidified sample and reductant) on the piezoelectric transducer, with the possibility of flow rate adjustment, permits a wide variation of sensitivity. The vapor-phase species were rapidly transported via a stream of Ar carrier to an MIP–OES for simultaneous multi-element determination. A univariate approach and simplex optimization procedure was used to achieve optimized conditions and derive analytical figures of merit. Analytical performance of the ultrasonic nebulization system was characterized by determination of the limits of detection (LODs) and precision (RSDs) with the ultrasonic nebulizer/dual capillary system (USN/DCS) observed at 15 µL min^?1 flow rate. An improvement in detection limits was achieved compared with pneumatic nebulization. Detection limits are superior to conventional pneumatic nebulization of elements. The experimental concentration detection limits for simultaneous determination, calculated as the concentration giving a signal equal to three times of standard deviation of the blank (LOD, 3σ_blank criterion, peak height), were 2.49, 1.75, 3.39, 2.13, 4.80, 6.21, 4.26, 2.01, 7.65, 3.92, and 4.65 ng mL^?1 for Au, Ag, Cd, Cu, Mn, Ni, Pb, Pd, Pt, Rh, and Zn, respectively. The method offers relatively good precision (RSD ranged from 8 to 12%) for liquid analysis and microsampling capability. The accuracy of the method was verified by the use of digested certified reference materials (NRCC TORT-1, NIES CRM-13, NIST SRM 2710, INCT SBF-4) and by aqueous standard calibration technique. The measured elements content in reference materials was in satisfactory agreement with the certified values.     

Flame Furnace Atomic Absorption Spectrometry: A Review

Abstract

Flame atomic absorption spectrometry (FAAS) is one of the most widespread traditional analytical techniques for trace element determination, but it often suffers from poor sensitivity due to the low nebulization efficiency and the short residence time of free atoms in the flame. On the basis of conventional FAAS, flame furnace atomic absorption spectrometry (FF-AAS) is developed with a tube (flame furnace) placed on top of the FAAS burner for the atomization. Sample is introduced via beam injection (BIFF-AAS) or thermospray (TS-FF-AAS). Due to the total sample introduction and prolonged residence time of free atoms in the flame furnace, marked sensitivity improvement is obtained for volatile and semivolatile elements over conventional FAAS. TS-FF-AAS can be employed as an element-selective detector for GC, HPLC, or CE for studying of metal speciation analysis and metallomics. In addition, three newly developed sample introduction methods, including ultrasonic nebulization, hydride generation, and pneumatic nebulization, are discussed. The analytical figures of merit and practical applications of FF-AAS in analytical atomic spectrometry are reviewed in this article.     

微波等离子体炬离子／原子荧光光谱研究：稀土元素铕的离子／？…

文中用微波等离子体炬作离子／原子化器,强短脉冲供电空心阴极灯作激发源,进行了稀土元素的离子／原子荧光检测。详细研究了系统对Ｅｕ检测时的最佳工作条件,对微波等离子体功能,空心阴极灯电流,观测高度等因素对Ｅｕ离子／原子荧光信号的影响进行了讨论测量了离子荧光和原子荧光谱的检测限。     

车轮轮辋缺陷的超声相控阵检测系统研究*

针对火车车轮检测中常规超声波探伤存在的检测灵敏度低、声束灵活性差、信噪比低等问题,研究了超声相控阵在火车车轮轮辋检测中的应用。本文介绍了超声相控阵检测技术的原理,并从超声相控阵换能器、硬件系统和软件系统三个方面阐述了火车车轮轮辋缺陷的超声相控阵检测系统的研究过程。最后通过人工模拟缺陷的相控阵检测实验,测试了该检测系统的性能,验证了相控阵检测设备具有灵敏度高、声束可控性好和可靠性高等优点。     

Analytical Evaluation of an Integrated Ultrasonic Nebulizer-hydride Generator System for Simultaneous Determination of Hydride and Non-hydride Forming Elements by Microwave Induced Plasma Spectrometry

ABSTRACT

The commercial ultrasonic nebulizer NOVA-DUO (ultrasonic nebulizer dual capillary system USN/DCS) has been evaluated for the simultaneous determination of classical hydride forming (As, Bi, Ge, Sb, Se, Sn) and conventional non-hydride forming (Ba, Ca, Fe, Li, Mg, Sr) elements by microwave induced plasma-optical emission spectrometry (MIP-OES). Simultaneous mixing and nebulization of the two solutions (acidified sample and reductant) on the piezoelectric transducer, with the possibility of flow rate adjustment, permits a wide variation of sensitivity. The hydrides and aerosols were rapidly transported via a stream of Ar carrier to a MIP for simultaneous multi-element determination by OES. A univariate approach and simplex optimization procedure was used to achieve optimized conditions and derive analytical figures of merit. Analytical performance of the ultrasonic nebulization system was characterized by determination of the limits of detection (LODs) and precision (RSDs) with the USN/DCS observed at 11 µL min^?1 flow rate. The experimental concentration detection limits for simultaneous determination, calculated as the concentration giving a signal equal to three times of standard deviation of the blank (LOD, 3σ_blank criterion, peak height) were 1.3, 5.9, 6.6, 1.8, 3.6, 2.6, 41, 8.1, 11, 7.5, 9.2, and 12 ng mL^?1 for As, Bi, Ge, Sb, Se Sn, Ba, Ca, Fe, Li, Mg, and Sr, respectively. The method offers relatively good precision (RSD ranged from 9 to 13%) for liquid analysis and microsampling capability. Interference effects by transition metals have been shown to be corrected by the addition of thiourea, as a pre-reducing agent and masking agent. The accuracy of the method was verified by the use of certified reference materials (NRCC DOLT-2, NRC GBW 07302, NIST SRM 2710, NIST SRM 1643e) and by aqueous standard calibration technique. All results obtained for reference materials were in agreement with certified values at 95% confidence level by Student t-test.     

用Monte Carlo模拟方法研究ICP－AES中的物理化学过程──Ⅰ．雾化过程的模拟

本文讨论了用ＭｏｎｔｅＣａｒｌｏ方法模拟ＩＣＰ－ＡＥＳ中雾化过程的理论依据和基本思想，得到的雾化效率与实验结果比较吻合。     

The development of recent high-power ultrasonic transducers for Near-well ultrasonic processing technology

With the reduction of crude oil throughout the world, enhance oil recovery technology has become a major oil research topics, which can greatly increase the recovery ratio of the crude oil before the dawning of renewable energy era. Near-well ultrasonic processing technology, as one new method, has attracted more attention for Enhanced Oil Recovery due to its low cost, good applicability and no environmental pollution in recent rears. There are two important relevant aspects about Near-well ultrasonic processing technology: (a) how to enhance the oil flow through the rocks into the pumping pool and (b) how to reduce the oil viscosity so that it can be easier to pump. Therefore, how to design a high-power ultrasonic equipment with excellent performance is crucial for Near-well ultrasonic processing technology. In this paper, recent new high-power ultrasonic transducers for Near-well ultrasonic processing technology are summarized. Each field application of them are also given. The purpose of this paper is to provide reference for the further development of Near-well ultrasonic processing technology.With the reduction of crude oil throughout the world, enhance oil recovery technology has become a major oil research topics, which can greatly increase the recovery ratio of the crude oil before the dawning of renewable energy era. Near-well ultrasonic processing technology, as one new method, has attracted more attention for Enhanced Oil Recovery due to its low cost, good applicability and no environmental pollution in recent rears. There are two important relevant aspects about Near-well ultrasonic processing technology: (a) how to enhance the oil flow through the rocks into the pumping pool and (b) how to reduce the oil viscosity so that it can be easier to pump. Therefore, how to design a high-power ultrasonic equipment with excellent performance is crucial for Near-well ultrasonic processing technology. In this paper, recent new high-power ultrasonic transducers for Near-well ultrasonic processing technology are summarized. Each field application of them are also given. The purpose of this paper is to provide reference for the further development of Near-well ultrasonic processing technology     

Advances in ultrasonic production units for enhanced oil recovery in China

With the development of oil recovery technology, ultrasonic technology has been involved in oil production and oilfield development. The mechanism of ultrasonic wave plugging in near well is different from the conventional oil recovery technology. Ultrasonic oil production technique is an effective method to enhance oil production with low cost, good applicability, and no environmental pollution. The core part of ultrasonic oil production equipment for Enhanced Oil Recovery is a high-power ultrasonic transducer. The continuous high-power ultrasound is used to treat the reservoir, which changes the pore structure, the physical property and the state of the fluid, thus improving the permeability and flows conditions of the reservoir, and increasing the oil yield and oil recovery. Ultrasonic oil recovery equipment includes the generation of high-power ultrasonic signals, long-distance transmission and the conversion of electrical energy to acoustic energy. In this paper, state-of-the-art on the development of ultrasonic oil production devices for Enhanced Oil Recovery in China is introduced. The purpose of this paper is to provide a reference for the development of high-power ultrasonic oil extraction equipment and its promotion in tertiary oil recovery technology.     

Experimental study of light diffraction by standing ultrasonic wave with cylindrical symmetry

We report a new acousto-optic arrangement based on ultrasonic wave with cylindrical symmetry. The theory of light interaction with standing cylindrical ultrasonic wave is experimentally verified in the Fraunhofer region. A very good agreement of experimental results with numerical calculations based on the proposed theory is found. The diffraction pattern consists of ring-shaped diffraction orders which posses a fine structure. The time average light intensity of the whole zeroth diffraction order as a function of the Raman-Nath parameter is investigated. The modulation properties of presented system are examined by means of single photon counting technique. Finally, some potentially useful applications in the laser and fibre technology are suggested.