Spark SSMS

SRM. selected reaction monitoring SSMS. spark source mass spectrometry... 

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. 

Although SSMS cannot be considered a surface technique due to the 1-5 rm penetration of the spark in most materials, few other techniques can provide a trace elemental survey analysis of surfaces consisting of films or having depths of interest... 

Due to the relative uniformity of ion formation by the RF spark (although its timing is erratic), the most widely used method of quantitation in SSMS is to assume equal sensitivity for all elements and to compare the signal for an individual element with that of the total number of ions recorded on the beam monitor. By empirically calibratii the number of ions necessary to produce a certain blackness on the plate detector, one can estimate the concentration. The signal detected must be corrected for isotopic abundance and the known mass response of the ion-sensitive plate. By this procedure to accuracies within a factor of 3 of the true value can be obtained without standards. 

Because GDMS can provide ultratrace analysis with total elemental coverage, the technique fills a unique analytical niche, supplanting Spark-Source Mass Spectrometry (SSMS) by supplying the same analysis with an order-of-magnitude better accuracy and orders-of-magnitude improvement in detection limits. GDMS analy-... 

Principles and Characteristics The original idea of spark-source mass spectrometry (SSMS) is due to Dempster [356], long before the first commercial instruments. In spark-source MS, atomisation and ionisation... 

SSMS can be classified among the milliprobe techniques (Figure 8.3), i.e. it is a unique link between microprobe techniques and macroanalytical methods that are characterised by poor lateral and in-depth resolutions (as in OES), or that have no lateral resolution whatsoever (as in NAA). Also, the achievable precision and accuracy are poor, because of the irreproducible behaviour of the r.f. spark. Whereas analysis of metals, semiconductors and minerals is relatively simple and the procedures have become standardised, the analysis of nonconducting materials is more complex and generally requires addition of a conducting powder (e.g. graphite) to the sample [359]. Detection limits are affected by the dilution, and trace contamination from the added components is possible. These problems can be overcome by the use of lasers [360]. Coupled with isotope dilution, a precision of 5% can be attained for SSMS. 

Applications Real applications of spark-source MS started on an empirical basis before fundamental insights were available. SSMS is now considered obsolete in many areas, but various unique applications for a variety of biological substances and metals are reported. Usually, each application requires specific sample preparation, sparking procedure and ion detection. SSMS is now used only in a few laboratories worldwide. Spark-source mass spectrometry is still attractive for certain applications (e.g. in the microelectronics industry). This is especially so when a multi-element survey analysis is required, for which the accuracy of the technique is sufficient (generally 15-30% with calibration or within an order of magnitude without). SSMS is considered to be a... 

Actinide metal samples are characterized by chemical and structure analysis. Multielement analysis by spark source mass spectrometry (SSMS) or inductively coupled argon plasma (ICAP) emission spectroscopy have lowered the detection limit for metallic impurities by 10 within the last two decades. The analysis of O, N, H by vacuum fusion requires large sample, but does not distinguish between bulk and surface of the material. Advanced techniques for surface analysis are being adapted for investigation of radioactive samples (Fig. 11) ... 

Because of the very important role of impurities in determining semiconductor properties, it is desirable to know their concentrations, at least of the electrically active ones. Of course, the techniques we have discussed in this chapter never make a positive identification of a particular impurity without confirmation by one of the established analytical techniques, such as spark-source mass spectroscopy (SSMS) or secondary-ion mass spectroscopy (SIMS). Once such confirmation is established, however, then a particular technique can be considered as somewhat of a secondary standard for analysis of the impurity that has been confirmed. It must be remembered here that an analytical method such as SSMS will see the total amount of the impurity in question, no matter what the form in the lattice, whereas an electrical technique will see only that fraction that is electrically active. 

In 1977, Jochum et aZ.12,14 developed the multiple ion counting (MC) technique using an old spark source mass spectrometer with 20 separate channeltrons 1.8 mm wide for simultaneous electrical ion detection. The sensitivity was increased by a factor of 20 compared to SSMS with ion detection using a photoplate and the precision of the analytical results was improved. 

Table 9.4 Result of trace analysis of high purity indium and zinc measured by spark source mass spectrometry (SSMS) and glow discharge mass spectrometry (GDMS), respectively.

SSMS - spark source mass spectrometer Mattauch-Herzog geometry ( / 10000). 

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