Spark-source ionization

Spark (source) ionization. Occurs when a solid sample is vaporized and partially ionized by an intermittent electric discharge. Further ionization occurs in the discharge when gaseous atoms and small molecular moieties interact with energetic electrons in the intermittent discharge. It is recommended that the word source be dropped from this term. 

The dynamic range of photographic detection is smaller in comparison with electric registration. However, the values for precision and accuracy found are more suitable than those noted for single ion monitoring (p. 27) and are comparable to results from spark source ionization. If a comparator, a data system and the suitable... 

Spark Source Mass Spectrometry (SSMS) is a method of trace level analysis—less than 1 part per million atomic (ppma)—in which a solid material, in the form of two conducting electrodes, is vaporized and ionized by a high-voltage radio frequency spark in vacuum. The ions produced from the sample electrodes are accelerated into a mass spectrometer, separated according to their mass-to-charge ratio, and collected for qualitative identification and quantitative analysis. 

The spark source is an energetic ionization process, producing a rich spectrum of multiply charged species (Af/2, Af/3, Af/4, etc.). These masses, falling at halves, thirds, and fourths of the unit mass separation can aid in the positive identification of elements. In Figure 2, species like Au and are labeled. The most abundant... 

Spark source mass spectrometry is used for the examination of non-volatile inorganic samples and residues to determine elemental composition. An RF spark of about 30 kV is passed between two electrodes, one of which may be the sample itself, causing vaporization and ionization. Powdered samples or residues from ashed organic materials can be formed into an electrode after mixing with pure graphite powder. 

Carbide cluster ions (MC + - M = matrix element) have been measured by investigating them directly from the solid carbides (B4C,46 SiC) or by analyzing metal oxide/graphite mixtures (for M = rare earth element,3 Si,46 Th or U36). Figure 9.60 shows the distribution of silicon carbide cluster ions (SiC +) in laser ionization mass spectrometry by the direct analysis of compact SiC in comparison to the carbide cluster ion distribution of LaC + and SrC + in spark source mass spectrometry, by investigating a metal oxide/graphite mixture. 

Spark source (SSMS) and thermal emission (TEMS) mass spectrometry are used to determine ppb to ppm quantities of elements in energy sources such as coal, fuel oil, and gasoline. Toxic metals—cadmium, mercury, lead, and zinc— may be determined by SSMS with an estimated precision of 5%, and metals which ionize thermally may be determined by TEMS with an estimated precision of 1% using the isotope dilution technique. An environmental study of the trace element balance from a coal-fired steam plant was done by SSMS using isotope dilution to determine the toxic metals and a general scan technique for 15 other elements using chemically determined iron as an internal standard. In addition, isotope dilution procedures for the analysis of lead in gasoline and uranium in coal and fly ash by TEMS are presented. 

Isotope Dilution By Spark Source Mass Spectrometry. A unique and quite different approach to determining trace elements in solids, liquids, and gases uses the isotope dilution technique. This method has been operational for some time with mass spectrometers. Thermal ionization... 

Spark Source Mass Spectrometry. Another method for trace analysis probably should be mentioned and that is spark source mass spectrometry. In this technique, the sample in the form of a solid serves as an electrode and vapors, formed by sparking, are atomized and ionized to metal ions which are separated by a mass spectrometer and measured. The equipment is expensive and good results require the attention of a skilled operator. Even under the best conditions order of magnitude agreement of results is about the best that can be achieved. 

As mentioned, thermal ionization mass spectrometry is the area in which isotope dilution developed and in which it has received the widest range of applications. One of thermal ionization s major limitations is that it is essentially a single-element technique in no way can it be considered multielement in the sense that numerous elements can be assayed in a single analysis. It is thus highly desirable to mate isotope dilution with multielement analysis capability. Spark source mass spectrometry for years dominated elemental analysis, but the nature of the samples (solids) made use of isotope dilution difficult. Use of a multielement spike was reported as long ago as 1970 by Paulsen et al. [17], however, and more recently by Carter et al. [18] and by Jochum et al. [19,20]. 

Four techniques based on mass spectrometry are widely used for multi-elemental trace analysis of inorganic compounds in a wide range of sample types. These techniques are thermal ionization (TI), spark source (SS), glow discharge (GD) and inductively coupled plasma (ICP) mass spectrometry. In these techniques, atomization and ionization of the analysed sample are accomplished by volatilization from a heated surface, attack by electrical discharge, rare-gas ion sputtering and vaporization in a hot flame produced by inductive coupling. 

In spark sources, electrical discharges are used to desorb and ionize the analytes from solid samples [98]. As shown in Figure 1.42, this source consists of a vacuum chamber in which two electrodes are mounted. A pulsed 1 MHz radio-frequency (RF) voltage of several kilovolts is applied in short pulses across a small gap between these two electrodes and produces electrical discharges. If the sample is a metal it can serve as one of the two electrodes, otherwise it can be mixed with graphite and placed in a cup-shaped electrode. 

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