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Another attempt to measure liquid samples was the coupling of a mini-in-torch vaporization ITV dry sample introduction system with an atmospheric pressure planar geometry microplasma device MPD [3] shown in Fig. Kaplan and F. Liquid sampling-atmospheric pressure glow discharge LS-APGD ionization source for elemental mass spectrometry: Preliminary parametric evaluation and figures of merit. Andrew D. Due to the very low frequency this plasma device should be allotted to the dielectric barrier discharges. Tech note. Virtual Conference. It was shown that the microchip plasma could be successfully applied for molecular emission detection. Best Paper Honorable Mention Award bib.❿
 
 

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This review describes several recent device geometries and provides a synopsis of the physics. Promising applications of this technology in chemical processing, lighting, water disinfection, and medicine are also discussed briefly. Manuela Miclea. This paper is an update on the development of microplasmas as detectors for gas chromatography.

Direct current dc , alternating current ac , and radio frequency rf microplasmas developed in recent years will be described with their significant analytical results, which mostly concern the detection of halogens and sulfur.

New results will be added which employ a microhollow cathode discharge MHCD as excitation source. Emphasis will be given to this microplasma which has already been implemented as an element-selective detector for emission spectrometry and as ionization source for mass spectrometry.

The possibility to use it as a multielement-selective detector for gas chromatography will be presented. A discussion of the published detection limits of all these microplasmas is given. Jan Eijkel. Gerardo Gamez. Jie Ge. WeiDong Zhu. Alin Eugen. Mark Tweedie. Andrew H Cannon. Ashish Sharma. UsMan KhAn. Sergei Kulinich. Jorgelina Altamirano.

Marin Senila. Jhanis J Gonzalez. Laifa Boufendi , G. Wattieaux , L. Meyer , C. Dirk Janasek. Robert Winkler. Patrick Chapon.

Pagona Papakonstantinou. Jerzy Mizeraczyk. Abdel-Aleam Hefney Mohamed. Journal of tissue engineering and regenerative medicine. Gilson Khang. Bernard Lacour. Vladimir Kolobov. Attila Bilgic. Jodi Shann. Dirk Vangeneugden.

Stephane Esnault. Fred Adams. Thierry Dufour. William Zimmerman. Caixiang Zhang. Log in with Facebook Log in with Google. Remember me on this computer. Enter the email address you signed up with and we’ll email you a reset link. Need an account? Click here to sign up. Download Free PDF. Analytical Detectors Based on Microplasma Spectrometry. Abstract Miniaturizing all dimensions of apparatus, such as electronics and computers, is the current trend followed by scientists in various fields.

Related Papers. Advances in atomic emission, absorption and fluorescence spectrometry and related techniques. Atomic Spectrometry Update. Advances in atomic spectrometry and related techniques. Prospects in Analytical Atomic Spectrometry. Spectrochimica Acta Part B-atomic Spectroscopy The dielectric barrier discharge — a powerful microchip plasma for diode laser spectrometry. Spectrochimica Acta Part B-atomic Spectroscopy Spectroscopic characterization of a microplasma used as ionization source for ion mobility spectrometry.

Spectrochimica Acta Part B-atomic Spectroscopy The dielectric barrier discharge as a detector for gas chromatography. Analytical and Bioanalytical Chemistry Microplasma-based atomic emission detectors for gas chromatography.

Sample preparation, injection and manipulation are already reduced in dimensions. A great importance should be emphasised in assembly of small devices that are portable, use less analyte and produce as close as possible, the same results obtained as with commercially available classical devices.

Part of this effort is also endeavoured to development of microplasmas. The plasmas are sometimes irreplaceable detectors of molecular fragments or elements. The miniaturisation of plasmas brings the advantage of atmospheric pressure operation.

With a few exceptions, most of them operate at atmospheric pressure. Due to the confinement in small volumes, they have significantly higher gas tem- perature compared to the non-thermal low pressure plasmas. By reducing the dimensions, the pressure has to increase. In order to ignite a plasma at atmospheric pressure, the distance between electrodes should be in the lm range. The extent of the implications of atmospheric pressure operation goes further than just reducing the dimensions.

At low pressure, the heavy particles temperature is much lower than the electron temperature and the collisions between electrons and heavy particles lead mostly to excitation and ionization. In this way, the temperature of heavy particles cannot rise too much. By increasing the pressure, the mean free path of the electrons and heavy particles is decreased, hence the frequency of collisions is increased.

This leads to more frequently inelastic collisions between electrons and heavy particles, inducing an efficient energy exchange between the plasma species. This induces higher plasma chemistry. The elastic collisions grow at higher pressures, leading to an increase in the heavy particles temperature. The plasma state is closer to the local thermal equilibrium but without reaching it. The density of excited species, especially metastable states, also increases with the pressure.

Some other favourite processes appear, for example, the three body collisions leading to the formation of dimer molecules. These molecules emit UV radiation which signifi- cantly contributes also to the plasma chemistry. The purpose of this review is to aid the reader to get an overview of plasma miniaturization in analytical spectrometry with the advantages and sometimes the problems encountered upon this development.

Some miniaturized plasmas will be described and their significant analytical performances will be presented. It is impossible to cover all microplasmas developed in the last years; They can be obtained from the last reviews and references herein [2—5]. In this review only those microplasmas who have analytical results will be presented and mainly the use of microplasmas as optical emission detectors or as excitation and ionization source for gas chromatography and mass spectrometry will be mentioned.

Analytical Plasma Detectors Three types of plasmas namely the glow discharge GD , the microwave induced plasma MIP and the inductively coupled plasma ICP are the commonly used plasma sources in analytical spectrometry [6].

They are used as analytical detectors for solid, liquid and gaseous samples. For example, the GD is used for the analysis of solid samples due to the presence of heavy ions colliding with the cathode, which is normally the sample to be analyzed.

Liquid samples are analyzed with the ICP due to the high gas temperatures, up to K present in this type of plasma. This parameter enables the evaporation and dissociation of any kind of samples and it is also robust enough not to be greatly influenced by the presence of water.

The ICP is normally coupled either with mass or optical emission spectrometry. The MIP is mostly used for the detection of gaseous or volatile substances. In comparison with the ICP, it is not so hot but its properties are appropriate for the excitation of non- metals. It is already commercially implemented as detector for gas chromatography.

Various kinds of miniaturized plasmas were developed, starting with dc plasmas, low and high frequency plasmas. In the following, some significant microplasma sources will be briefly described and their most important analytical results will be presented. They can be classified in many ways, either by their function as excitation or ionization source optical emission or mass spectrometry detectors or by their operation conditions. A classification upon their frequency operation will be made in this paper.

Microplasmas for the Analysis of Gaseous Samples Direct Current Plasmas Glow Discharge on a Chip The first molecular emission detector on a glass chip, employing a miniaturized direct current helium plasma was reported by Eijkel et al. The electrodes were made of 50 nm chromium and nm of gold. The plasma was generated in chambers of different geometrical dimensions at a pressure of about hPa.

A chamber with a volume of 50 nl at a typical operating pressure of hPa was used as an excitation source. The lifetime of the device was limited to 2 h due to cathode sputtering. In a further paper Eijkel et al. One design of the plasma chip is shown in Fig.

The validity of the scaling theory was demonstrated by the creation of an atmospheric helium plasma in a nanoliter-size discharge chamber on a microchip. Chambers of volumes of The plasma was constricted in the channel and the current—voltage characteristic showed the operation in the GD regime. In this device, the dissociation and excitation of the analyte species occur by collisions with electrons and excited helium atoms. The detection of methane in the helium gas flow by measuring molecular bands of CH was tested.

In the case of low flow rates, the analytical signal was linear over two decades. It was shown that the microchip plasma could be successfully applied for molecular emission detection. It was also tested with some other organic compunds like propionic acid, triethylamine, benzylamine. The authors are claiming that the simple instrumentation, the small detector size and the good sensitivity make the device highly suitable for integration in microanalysis systems.

In the following paper, the same group coupled the plasma chip described above to a conventional gas chromatograph, in order to investigate its performance as an optical emission detector [9]. The plasma was generated in helium and the applied power was 9 mW V, 12 lA. A number of carbon-compounds were detected in the column effluent, recording the CO-emission at nm.

However, all components of the chromatogram showed considerable broadening and tailing. The authors proved that these effects were not related to the performance of the plasma but to dead volumes in the connection tubes and the channels of the glass chip. It can be expected that the integration of the chromatographic column and the plasma detector on a single chip reduces the dead volumes and improves the signals.

The device was operated for more than 24 h without a significant change in performance. The operation is stable and instrumental requirements are simple. Atomic detection of halogens bromine and chlorine was reported by Bessoth et al.

The design presented in Fig. The plasma is ignited between a pair of electrodes in the channel. The plasma was operated at atmospheric pressure with powers of about mW. Windows were cut on the top electrode so that optical emission could be monitored using a fiber optic spectrometer. Helium background spectra of this self-igniting plasma and relatively low excitation temperatures between K and K using He lines were reported at atmospheric and sub-atmospheric pressure operation.

A cooling of the chip was reported to be necessary at power levels above 10 W although typical power levels were between 1 W and 3 W. In addition, a CCP was also used to improve by plasma treatment the surface of the inner wall of polymeric capillaries for use in capillary electrophoresis applications [31]. Capacitively Coupled Microplasmas, There are only few publications on this plasma Fig.

Some patents [33, 34] and a PhD thesis [35] report about the implementation of this microplasma as an emission detector for GC. The capacitively coupled plasma consists of two disc shaped electrodes made of gold deposited on tungsten. These two electrodes are separated by an insulator disc made of ruby, sapphire or ceramic. All three discs have a hole. The plasma is confined in the hole of the ceramic piece which has a diameter between lm and lm.

The thickness of the ceramic is about lm. The three discs are pressed together in order to ensure that helium plasma gas is flowing only through the hole. The plasma is operated at The power coupled into the discharge is between 10 W and 15 W. The plasma was developed as multielement detector for gas chromatography.

The GC column is placed directly in front of the lower disc elec- trode. The analytical results with this microplasma show the detection of chlorinated compounds with a detection limit for Cl of 8.

The detection limits for some other halogens like F, Br and also S are presented in the pg range. Inductively Coupled Plasmas, It was found that the electron density increases with the frequency and is about an order of magnitude higher than in a large scale ICP due to the large surface to volume ratio of small discharges. The motivation for the work was to develop portable mICPs that can be coupled to a microfabricated Fabry—Perot interferom- eter for measurement of gaseous analytes, for example SO2 in the field [42—46].

The first generation of mICPs were developed with load coil diameters of 5, 10 and 15 mm and operated with powers of 0. These proof-of-concept devices were developed on printed circuit boards to study the effect of scaling laws on mICPs [38]. Such studies formed the foundation for further developments. For instance, for the next two generations, photolithography and micromachining technology were used for fabrication of mICPs that had planar load coils shown in Fig.

A matching network was also microfabricated next to the load coil [48]. A one-mask fabrication process was used for the matching network and the mICP fabrication, thus reducing cost by alleviating the need for mask alignment as would be required if multiple masks were used [38— 40].

Another paper reports on the microfabrication and testing of monolithic mICP, fabricated on glass wafers using surface micromachining [41]. The plasma is sustained by coupling a MHz current into a low pressure gas. Ar as well as air plasmas have been generated in the range 0. The operation power was mW, although 1.

In this case the coil was situated closer to the plasma and was operated with even higher frequencies up to MHz. The plasma chamber consisted of a cylindrical hole of 6 mm diameter and 6 mm in length.

The pressure was 7. Microwave Induced Plasmas, MHz—2. This microstrip plasma source MSP consists of a single 1. The electrodeless plasma is operated at atmospheric pressure, with a microwave input power of 5—30 W. It has the potential to become very useful in analytical chemistry for the emission detection of non-metals like halogens and chalcogens.

Bilgic et al. Microstrips were used for power transmission and produced by plasma vapor deposition with a subsequent sealing by galvanic covering with copper, up to a thickness of about 1 lm. The latter passes the skin depth of microwaves at a 2. The underlying copper block has a thickness of up to 1 cm and acts both as a ground electrode and a cooling medium.

The micro- strip has a sidearm acting as an artificial load. Its length is selected so that fluctua- tions in the plasma load, e. The device, of which the novel aspects are described in [51], could be operated for hours without any deterioration of the microstrips or of the channel in the quartz.

It could be used with 0. For leachates of soils, accurate determinations of traces of mercury were shown to be possible. This plasma was shown to be able to break down halogenated hydrocarbons and in atomic emission signals for the Cl I The plasma configuration could also be modified so that the plasma exits from the chip, which however requires an adaptation of the matching element length. Then, the space angle in optical emission work is no longer limiting.

At a power of 30 W and with an argon flow of 0. A further stable microstrip microwave plasma MSP operated at atmospheric pressure with a power of some 10—20 W and at a gas flow of 0. The development of a new, very small coaxial plasma source based on a micro- wave plasma torch MPT is described [56]. It also works well with helium and does not show any wear during a test period of 30 h of operation with argon.

It is, in particular, thought to be a source for the atomic spectrometry of gaseous species. The excitation temperature is found to be about K for this device operating with helium and 17 W microwave power. A detection limit for an example application in which Cl is detected from HCCl3 is found to be below 66 ppb. The design considerations for the microstrip circuits are discussed and an approximated calculation for the layout is presented.

With the introduced proce- dure, it is possible to design even smaller MPTs for special applications. The plasma device is shown schematically in Fig. Argon and air discharges can be self-started with less than 3 W in a relatively wide pressure range. An ion density of 1. Atmospheric discharges can be sustained with 0. This low power allows for portable air-cooled operation.

Continuous operation at atmospheric pressure for 24 h in ar- gon at 1 W shows no measurable damage to the source. The application of microplasmas as sensors of industrial vacuum processes requires stable operation at gas pressures of less than 1 Pa [58]. Using atomic emission spectrometry, the detection of helium in air is found to have a detection limit of ppm, which is three orders of magnitude worse than the DL of SO2 in argon.

The loss of sensitivity is traced to the high excitation energy threshold of He and to the poor ionization efficiency inherent in air plasma.

At atmospheric pressure, a microdischarge is generated in a 25 lm-wide gap in a microstrip transmission line resonator operated at MHz.

The volume of the discharge is 10—7 cm3, and this allows an atmospheric air discharge to be initiated and sustained using less than 3 W of power. The thermal characteristics of an atmospheric argon discharge generated with a low-power microwave plasma source are investigated to determine its possible integration in portable systems. Rotational, vibrational, and excitation temperatures are measured by means of atomic emission spectrosmety [59]. It is found that the discharge at atmospheric pressure presents a rotational temperature of K, while the excitation temperature 0.

Therefore, the discharge is clearly not in thermal equilibrium. The low rotational temperature allows for an efficient air-cooled operation and makes this device suitable for portable applica- tions, including those with tight thermal specifications, such as treatment of biological materials.

The difficulty starts to appear when trying to analyze liquid samples for different reasons. First of all, the introduction of liquid samples in form of aerosols is difficult because the dimensions of the plasmas are very small. Even if such a miniaturized device would exist, its efficiency is reduced.

Secondly, for miniaturized plasmas, the volume and discharge power is such that even small amounts of liquid can easily extinguish the discharge. The increase of the plasma power over a certain limit 20— 30 W is not possible due to the strong thermal stress by a extremely high power density. However, some developments of microplasmas that are able to analyze liquid samples were investigated and they will be presented in the following. A miniaturized atmospheric-pressure thermal plasma jet source shown in Fig.

The plasma source design required for achieving higher power transfer efficiency to the plasma has been studied mainly so that it can be operated with a commercially available compact VHF transmitter.

The plasma was powered from a commercially available — MHz transmitter. The maximum output power was 50 W. The power losses to the matching network were addressed. A selection of dielectric material was sorted out and the antenna thickness and number of turns for the load coil were examined.

By these parameters the authors studied the effect of gas flow rate on plasma density and measured excitation temperatures using a Boltzmann plot of Ar lines. Overall, plasma density was reported to increase up to cm—3 and excitation temperatures ranged between K and K.

The use of an electrospray biased at 3 kV , sample introduction was reported to be easier and emission signals from a ppm NaCl solution were obtained. A sharp emission peak of Na I was clearly observed at nm, when the sample solution was introduced, while Fig. A detection limit of 5 ppm has been attained. Another attempt to measure liquid samples was the coupling of a mini-in-torch vaporization ITV dry sample introduction system with an atmospheric pressure planar geometry microplasma device MPD [3] shown in Fig.

This mini-ITV consists of a sample carrying probe formed by five turn coiled filament, made from Re, secured on a ceramic support, and a small volume vaporizer chamber with a carrier-gas inlet. The sample was dried with a low power and the outlet of the vaporization chamber was connected to the inlet of the MPD. A higher electrical power was supplied in order to vaporize the residue that remains on the coil. The vaporized sample was carried to the MPD by Ar carrier gas and it was dissociated and detected by optical emission spectrometry.

The detection of Li was reported with a detection limit at least better than 30 ppb. Another discharge source, known as the electrolyte as a cathode discharge ELCAD , has received some attention and may have potential as a detector for l- TAS. The sample solution is electrically connected to the negative electrode such that the overflowing liquid surface becomes the discharge cathode [60].

Emission spectros- metry of metal analytes in the electrolyte solution has been performed in air at atmospheric pressure using this technique and the authors suggest the cathodic sputtering as being the key mechanism of sample transport from the liquid to gas phase. A relationship between pH and spectral line intensity was interpreted as being due to a reaction between hydroxonium ions and solvated electrons leading to an increase in the secondary electron emission coefficient.

This in turn reduces the Fig. Acidification of the sample solution is thus applied to most ELCAD sources to increase sample transport into the discharge. It has been developed by Marcus and Davis, in which the electrolyte sample flows through a stainless steel capillary connected to the negative electrode and a GD ignited between capillary and a metal anode [61].

The authors cite thermal vaporization of the sample by Joule heating as being the key mechanism of sample transport into the discharge. The plasma can operate with liquid flow rates of 0. A special optical arrangement was used to image the plasma into the spectrometer. The detection limits in this case are, for example, for Na 1 ng while for Hg is 15 ng. The first attempt used a micro-fluidic device fabricated in glass and ignited a GD between a sample stream flowing within a micro-channel and a metal anode [63].

Argon gas entering from another micro-channel set up a flowing liquid—gas interface within the device to allow ignition of the discharge. However, discharge instabilities occurred due to the high gas temperature. An improved device is presented in Fig. Operation in air, instead of argon is also demonstrated. Further miniaturization of the inlet channel dimensions indicates the potential for coupling such a detection system with other l-TAS elements.

A preliminary absolute detection limit of 17 nmol s—1 is obtained for Na with a flow rate of ll min—1 and using a ms spectrometer integration time. Wilson and Gianchandani developed an atmospheric pressure glow micro-dis- charge fabricated on a glass substrate.

In this device, shown in Fig. A GD is ignited between a patterned metal electrode and the sample solution, which is in contact with a patterned metal cathode. Emission spectrometry Fig. The LEd-SpEC device was shown to detect sodium impurities of concentration less than 10 ppm, lead impurities at 5 ppm, and aluminum and chrome impurities of 10 ppm.

However, the static nature of the sample droplet and large dimensions would be problematic, if integration with other l-TAS copartments is desired. More recently, a novel device shown in Fig. Once a gap has been established, the voltage applied is high enough to cause electrical breakdown, generating a discharge in the sample vapors and allowing emission spectrosmetry to be performed.

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Click here to sign up. The first generation of mICPs were developed with load coil diameters of 5, 10 and 15 mm and operated with powers of 0. William Zimmerman. The LEd-SpEC device was shown to detect sodium impurities of concentration less than 10 ppm, lead impurities at 5 ppm, and aluminum and chrome impurities of 10 ppm. At atmospheric pressure, a microdischarge is generated in a 25 lm-wide gap in a microstrip transmission line resonator operated at MHz.

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