一种原子光谱分析用新激发光源——千瓦级微波等离子体炬(kW-MPT)

Based on the simulation of transmission and distribution characteristics of the electromagnetic field inmicrowave plasma torch(MPT) torches with different configurations using electromagnetic simulation software and experimental study, a new MPT torch with double resonant configuration was, for the first time, developed. The results show that the inner tube of MPT torch plays an important role in strengthening the electric field intensity at the open end of the MPT torch and redistributing the electromagnetic field in the whole torch by the formation of the double resonance. It contributes also to enhance the macroscopic stability and the self-sustaining of the plasma. The stability of the plasma was shown to be excellent when the spacer between inner and intermediate tubes is located about 20—30 mm from the top opening of the torch. Preliminary study showed that the analytical performance for 13 common elements was approaching that of traditional ICP-AES.     

微波等离子体炬耦合方式的研究

采用气动雾化连续进样、端视观测法,考察了微波等离子体炬原子发射光谱法中等离子体Ar线的背景发射以及Al,Mg,V等元素的信号发射强度随天线耦合连接点位置的不同而发生的变化.结果表明,当天线位于炬管顶端,即天线距离活塞3λ/4和λ/4时均能获得较好的等离子体,λ/4略好,信号发射强度和信背也较大,只是精密度略差一些.初步探讨了MPT炬管的电磁场结构.     

A versatile new torch for inductively coupled plasma spectrometry

A modified torch for optical emission spectrometry with an inductively coupled plasma source is described. The demountable torch incorporates a flared intermediate tube, a capillary injector tube and interchangeable jets at the gas inlets. The optimised performance of the torch is compared with that of a conventional torch. The new torch can be operated over a wide range of gas flows and shows considerable promise in work with an argon-cooled plasma. The ability to operate at high or low gas flow rates, and the possibility of interchanging tubes and jets easily illustrate the versatility of the new design.     

An improved microwave plasma torch for atomic spectrometry

The analytical performance of a microwave plasma torch was improved through mechanical alterations. Several problems reported in earlier designs were addressed: the ignition and stabilization of a helium plasma in the MPT was difficult; high powers were required to both ignite and operate the plasma; otherwise, the plasma would erratically change from an annular to a filament type discharge. In the new torch, the helium discharge was stabilized by replacing the copper central tube with one made of quartz. In addition, air entrainment was alleviated through use of a sheathing gas. This modification simplified the background mass spectrum and raised the effective ionization temperature of the discharge. A detailed schematic diagram of the new microwave plasma torch is presented.     

气动雾化进样时微波等离子体炬作为激发光源的性能研究

以气动雾化进样研究了微波等离子体炬（ＭＰＴ）放电作原子发射光谱法激发光源的性能，包括ＭＰＴ的获得、操作参数的影响、样品引入及其分析性能，并与微波诱导等离子体进行了比较，证明ＭＰＴ放电作激发光源有良好的分析性能．     

Modeling of RF plasma torch with a metallic tube inserted for reactant injection

Flow, temperature, and electromagnetic (EM) fields in a radio-frequency thermal plasma torch designed for the preparation of superconducting powders or films have been analysed by using a new two-dimensional modeling approach with the electric field intensity as the fundamental EM field variable. The insertion of a stainless steel injection tube into the torch leads to large induction currents in this tube. Although such large induction currents cause pronounced changes of the EM fields near the injection tube, flow and temperature fields are little affected. There exists only one large toroidal vortex in the upper part of the present torch, while the maximum temperature appears at an off-axis location within the coil region.     

Microwave plasma torch mass spectrometry for some rare earth elements

Rare earth elements (REEs) have been widely applied in modern industry and material science due to their special chemical properties and luminescence properties, but their environment pollution problem has also attracted attention. How to trace and control impact of REEs on environment and develop highly sensitive methods for REEs analysis have practical significance. Microwave plasma torch (MPT) is a kind of simple, low power consumption (～200 W) and easily operated plasma generators. When it was coupled with varied mass spectrometers as ion source of mass spectrometry (MS), i.e. MPT-MS can use for the analysis of metal elements in aqueous with the remarkable advantage of only minimal or even no simple pretreatment, and can meet comprehensive requirements of environmental control and water quality monitoring. MPT-MS have also an ability to carry out online real-time monitoring and analysis of water environment. Compared with the traditional ICP-MS, it can obtain more effective information and has higher sensitivity (the detection limit is at sub-ppb level). This paper reviews common methods and research progress of REEs analysis in recent years. Practical applications and advantages of MPT in the analysis of REEs are briefly summarized. Specifically, this paper introduces some work recently done in our group on analysis of REEs by the MPT, including analysis of metal elements distribution in water samples in local Poyang Lake, and general rules of formation and behavior of complex metal ions in the MPT plasma are also proposed afterwards. Through the practically dealing with the Poyang Lake case by the MPT, hopefully this would interest more academia into this area so as to speed up development of the MPT itself.     

Microwave plasma torch mass spectrometry for the direct detection of copper and molybdenum ions in aqueous liquids

Microwave plasma torch (MPT) is a simple and low power‐consumption ambient ion source. And the MPT Mass spectra of many metal elements usually exhibit some novel features different from their inductively coupled plasma (ICP) mass spectra, which may be helpful for metal element analysis. Here, we presented the results about the MPT mass spectra of copper and molybdenum elements by a linear ion trap mass spectrometer (LTQ). The generated copper or molybdenum contained ions in plasma were characterized further in collision‐induced dissociated (CID) experiments. These researches built a novel, direct and sensitive method for the direct analysis of trace levels of copper and molybdenum in aqueous liquids. Quantitative results showed that the limit of detection (LOD) by using MS² procedure was estimated to be 0.265 µg/l (ppb) for copper and 0.497 µg/l for molybdenum. The linear dynamics ranges cover at least 2 orders of magnitude and the analysis of a single aqueous sample can be completed in 5–6 min with a reasonable semi‐quantitative sense. Two practical aqueous samples, milk and urine, were also analyzed qualitatively with reasonable recovery rates and RSD. These experimental data demonstrated that the MPT MS is able to turn into a promising and hopeful tool in field analysis of copper and molybdenum ions in water and some aqueous media, and can be applied in many fields, such as environmental controlling, hydrogeology, and water quality inspection. Moreover, MPT MS could also be used as the supplement of ICP‐MS for the rapid and in‐situ analysis of metal ions. Copyright © 2016 John Wiley & Sons, Ltd.     

微波等离子体光谱技术的发展(二)

微波等离子体光源是一类重要的有较强激发能力的原子发射光谱光源,主要包括微波感生等离子体光源,电容耦合微波等离子体光源及微波等离子体炬光源。本文是微波等离子体光谱技术发展的第二部分,主要介绍了电容耦合微波等离子体光源及微波等离子体炬光源的结构原理和性能。并对它们的技术特点和进展进行评述。     

Transferred plasma jet as a tool to improve the wettability of inner surfaces of polymer tubes

The wettability of the inner surfaces of vinyl, polyurethane, and silicone tubes was modified using an atmospheric pressure plasma jet operated in argon. A specific plasma jet configuration, transferred plasma jet, developed at Sao Paulo State University was utilized. It has been shown that it is possible to homogeneously alter the inner wall wettability of 1-m-long tubes, while providing safe plasma source usage for the operator. The water contact angle for three tube materials, i.e., vinyl, polyurethane, and silicone, changed from 98°, 86°, and 109° to 55°, 45°, and 40°, respectively.     

Thermospray nebulizer as sample introduction technique for microwave plasma torch atomic emission spectrometry

A thermospray nebulizer was used as a sample introduction device for microwave plasma torch (MPT) atomic emission spectrometry (AES). Experimental parameters, including the power supplied to the MPT, the flow rates of support and carrier gases, the observation height, the sample uptake rate, the thermospray working temperature, the temperature of the aerosol spray chamber and cooling water were optimized. Under optimum conditions, the relative standard deviation (RSD) of 10 measurements for 21 elements is in the range 0.3–2.0%. The detection limits were improved in comparison with the ultrasonic nebulizer as sample introduction technique for MPT–AES. The inclusion of 20% methanol into the MPT showed there is no effect on the stability of MPT discharge. The technique can thus be held to have the potential for interface to reverse-phase HPLC systems.     

New design of a radio-frequency plasma torch

A numerical model has been developed for predicting the two-dimensional flow and temperature fields in a radio-frequency (rf) plasma torch. The method employed here is based on Boulos' model with the exception of the boundary conditions for the electric and magnetic field equations. Calculations have been made for the confirmation of a new sample injection method, which is capable of completely evaporating refractory materials at high feeding rates without interfering with the stability of the plasma. In the newly designed torch, the reagent is radially injected into the hottest part of the plasma through quartz capillary tubes set symmetrically between an inductor coil. Experimental investigations have also been performed for verifying the proper function of the design. These results provide evidence that our radial injection method developed here is more effective in practical processing than the conventional axial injection methods.     

Thermal imaging of microwave fields inside the surfatron and the microwave plasma torch

A new method is introduced for imaging microwave fields, such as those found in microwave-plasma support structures. The method relies upon the darkening that such fields cause in heat-sensitive paper, such as that used in some telefax printers. With this new method, the microwave-frequency electric fields inside two microwave-plasma support structures, the surfatron and the microwave plasma torch, have been measured and subsequently imaged in three dimensions. The images reveal that the surfatron and microwave plasma torch have different operational behavior. As expected, the electric field strength inside the surfatron exponentially falls off down the length of the quartz plasma tube. The field inside the microwave plasma torch initially diminishes, but then increases in strength towards the end of the tube. An aerosol was introduced into the surfatron to observe the effect of water vapor on the electric field strength and distribution. The exponential axial decay of the electric field in the ‘dry’ surfatron plasma, characteristic of a surface wave propagating down a quartz plasma tube, is extended further down the quartz tube in the ‘wet’ plasma. A drop in plasma conductivity is likely the origin of the elongated propagation of the surface wave.     

Three-dimensional morphological chirality induction using high magnetic fields in membrane tubes prepared by a silicate garden reaction

Using a vertical superconducting magnet (max. 15 T), we studied magnetic field effects on membrane tube morphology prepared by a silicate garden reaction. At zero field, semipermeable membrane tubes grew upward when metal salts were added to a sodium silicate aqueous solution. In the presence of a magnetic field (15 T, downward) right-handed helical membrane tubes grew along a glass vessel's inner surface when magnesium chloride and copper sulfate were added. Referring to membrane tubes by the names of metal cations used in their preparation, in the case of Mg(II) and Zn(II) membrane tubes, the left-handed helical tubes grew when the field direction was reversed upward. The left-handed helical Mg(II) membrane tubes grew in the magnetic field when a glass rod was placed in a vessel. Mg(II) and Zn(II) tubes, separate from a vessel wall, grew in a twisted shape in the magnetic field. In situ observation of the solution's motion during the reaction revealed that the Lorentz force on the outflow from the opened top of the hollow membrane tube induced convection of the solution near the tube exit, engendering chiral growth of the membrane tubes. Relative orientation of the outflow and a boundary (a vessel wall or glass rod surface) helped to determine the convection's direction.     

微波等离子体炬光源基本特性的研究

用计算机化断层扫描成象技术研究了微波等离子体炬(MPT)放电的发射轮廓,证明该光源具有良好的对称性,并有一个有利于样品引入的中央通道,最佳分析区在炬管上方5～10 mm,用激光Thomson散射和Rayleigh散射技术测定了ArMPT和HeMPT放电的电子温度、电子密度和气体温度,证明MPT放电的电子温度很高而气体温度较低,是一种非热光源。其中的高能电子处于过布居状态,具有很高的激发能力。     

用同轴表面波激励器和微波等离子体炬获得的微波等离子体的性能研究

同轴表面波激励器和微波等离子体炬是两种获得微波等离子体(MWP)的装置,本文比较了用这两种装置获得的MWP作原子发射光谱法光源时的分析性能,结果表明这两种装置各有优点,但微波等离子体炬效果更好。     

The electromagnetic performance of a surfatron-based coaxial microwave plasma torch

Low power microwave plasma torches are of particular interest to analytical chemists. The torch design investigated herein, called TPS, is based on the known surfatron structure to which a coaxial section is added consisting of an impedance transformer followed by the metallic nozzle at the tip of which the discharge occurs. A series of experiments illustrate the main electromagnetic features and performance of this novel coaxial microwave plasma torch operating at 2.45 GHz and with input power in the range 10–180 W. A specially devised slotted coaxial line with a movable probe arrangement can be inserted into the torch in place of the transformer section to provide in situ measurements of the plasma impedance. Analyzing these results, we show that the shape of the torch tuning characteristics can be controlled to improve the power transfer to the plasma and stability of operation with respect to changes in discharge conditions; under these conditions, the design of the device can be simplified. The procedures presented have a general character and can be applied to various torch configurations.     

Influence of the Shroud Gas Injection Configuration on the Characteristics of a DC Non-transferred Arc Plasma Torch

The characteristics of the plasma jet emanating from a dc non-transferred plasma torch is affected by many factors including arc current, type of gas, gas flow rate, gas injection configuration and torch geometry. The present work focuses on experimental investigation of the influence of shroud gas injection configuration on the I–V characteristics and electro-thermal efficiency of a dc non-transferred plasma torch operated in nitrogen at atmospheric pressure. The plasma gas is injected into the torch axially and shroud gas is injected through three different nozzles such as normal, sheath and twisted nozzles. The effects of flow rates of plasma/axial gas and arc current on I–V characteristics and electro-thermal efficiency of the torch holding different nozzles are investigated. The I–V characteristics and electro-thermal efficiency of the torch are found to be strongly influenced by the shroud gas injection configuration. The effect of arc current on arc voltage decreases with increasing the axial gas flow rate. At higher axial gas flow rate (>?45 lpm), the I–V characteristics of the plasma torch are similar irrespective of the nozzle used. The variation of electro-thermal efficiency with arc current is almost similar to that of arc voltage with arc current. As expected, the electro-thermal efficiency is increased when the axial gas flow rate is increased and at higher axial gas flow rate, it is not influenced by the arc current and shroud gas configuration. The plasma torch with normal nozzle may be better in the range of operating conditions used in this study.     

微波辅助在线分离富集Cd的初步研究

以７１７阴离子树脂为在线分离富集的柱填充材料,用微波等离子体炬原子发射光谱法（ＭＰＴ－ＡＥＳ）测定Ｃｄ,研究了施加微波对分离富集的影响。实验结果表明,施加微波明显有利于富集和脱过程,使Ｃｄ的发射强度明显增大。     

低功率微波等离子体炬原子发射光谱法的研究——超声雾化进样测定金、银、铂、铑、钯

本文提出一种测定贵金属元素的微波等离子体炬原子发射光谱法(MPTAES)。采用自制的超声雾化微量进样装置进样,以氩气为工作气体,探讨了观察高度,微波功率、体系介质、氩气流量和共存元素对被测元素发射信号的影响。选用合适的分析线和MPT光源的工作参数,其方法的检出限分别为5.8(Au)、0.5(Ag)、12(Pt)、1.6(Rh)和t 1.0ng/ml(Pd)。实际样品中金和银的测定结果是令人满意的。