Spark detection limit

Calibration of an arc or spark source is linear over three orders of magnitude, and detection limits are good, often within the region of a few micrograms per gram for elements such as vanadium, aluminum, silicon, and phosphorus. Furthermore, the nature of the matrix material composing the bulk of the sample appears to have little effect on the accuracy of measurement. 

Portable x-ray energy dispersive sulphur in oil analyser ASE-1 with measurement range 0.015 - 5% and a detection limit near 0.001%. SPARK-1-2M, BRA-17-02 and ASE-1 have been certified as measuring... 

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-... 

Approximately 70 different elements are routinely determined using ICP-OES. Detection limits are typically in the sub-part-per-billion (sub-ppb) to 0.1 part-per-million (ppm) range. ICP-OES is most commonly used for bulk analysis of liquid samples or solids dissolved in liquids. Special sample introduction techniques, such as spark discharge or laser ablation, allow the analysis of surfaces or thin films. Each element emits a characteristic spectrum in the ultraviolet and visible region. The light intensity at one of the characteristic wavelengths is proportional to the concentration of that element in the sample. 

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. 

Table 8.60 shows the main features of GD-MS. Whereas d.c.-GD-MS is commercial, r.f.-GD-MS lacks commercial instruments, which limits spreading. Glow discharge is much more reliable than spark-source mass spectrometry. GD-MS is particularly valuable for studies of alloys and semiconductors [371], Detection limits at the ppb level have been reported for GD-MS [372], as compared to typical values of 10 ppm for GD-AES. The quantitative performance of GD-MS is uncertain. It appears that 5 % quantitative results are possible, assuming suitable standards are available for direct comparison of ion currents [373], Sources of error that may contribute to quantitative uncertainty include sample inhomogeneity, spectral interferences, matrix differences and changes in discharge conditions. 

Arc/spark emission methods have been widely used for the determination of metals and some non-metals particularly as minor and trace constituents. In recent years, however, the technique has been extensively displaced by atomic absorption spectrometry, and plasma emission methods. Detection limits for many elements are of the order of 1-10 ppm (Table 8.3) and as... 

The GDL can be used for the analysis of trace, minor and major constituents in electrically conducting samples, especially metallurgical specimens. Similar detection limits to arc/spark methods are observed but with greater freedom from interferences and much improved precision (Figure 8.9). 

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) ... 

Mass spectroscopy Spark-source mass spectroscopy has been applied to certain terrestrial and lunar materials with excellent results because of its very low detection limit and the exactness of the results. Drawbacks are the cost of the instruments and the time needed for each analysis. 

---