Mass spectrometry spark source

The method of spark source MS was developed by Dempster in 1935 . During the last two or three decades, this technique was utilized in the trace analysis of impurities in high purity elements, such as semiconductors, superconductors, nuclear reactor components and magnetic, thermoelectric or luminescent materials. There is an urgent necessity for the determination of trace elements in these materials, because they are characterized by the presence or absence of particular elements in the ppm or ppb range. 

For several years, multi-element analysis of biological materials and environmental samples have been performed using spark source One example is the analy- 

Element IAEA Animal blood 66/12 UKAEC Mammalian blood (Mean values) 

As shown by this example, the samples mostly must be ashed (dry or wet) to prevent a superposition of metal ions and organic ions in the mass spectrum. Heavy metals such as Pt, Au, Hg, Tl, Pb and Bi have been detected from blood, homogenized liver and urine without prior ashing, in concentrations below 1 ppm . 

A higher accuracy of the results may be achieved by automatic evaluation of the photoplates, using an absolute calibration method working without standards . 

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 

Trace and ultratrace analysis SSMS, GD-MS, LA-ICP-MS, (IDMS) Chapter 8 

Isotope analysis TIMS, ICP-MS, SIMS, (IDMS) Section 8.5.4 

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 

Due to the low spatial and energetic spread of ions from TI, the method can be combined with single-focusing magnetic sector mass analyzers or quadrupoles [35], Nonetheless, TI ion sources require dedicated instrumentation, frequently equipped with multicollector (MC) systems to insure the highest accuray for the isotope ratios measured (Chaps. 3.3.2 and 7.2 in [3]). 

Note In the element MS community it is common to use the acronym TIMS without hyphen rather than the form TI-MS. The same is observed in case of other techniques employed for element MS, e.g., secondary ion mass spectrometry is abbreviated SIMS rather than SI-MS. 

The spark source (SS) developed by Dempster in 1935, provided the first truly multi-element and isotopic trace element method [40]. In spark source mass spectrometry (SS-MS), a solid sample is vaporized under vacuum by a high-voltage radiofrequency spark. The electric discharge is maintained between two pinshaped electrodes (about 10 mm in length and 1-2 mm in diameter) in vacuum. 

The detection limits for the elements from Rb through U generally vary between 0.001 and 0.1 ppm (equivalent to 0.001 to 0.1 pgg ). Certain elements 

Obviously, SS-MS is not suited for elemental analysis of small sample amounts, but SS-MS offers a high dynamic range making it very powerful for multiple element analysis including those present at trace level in alloys, ores, and similar samples. SS-MS also offers wide element coverage, an extensive concentration range and analysis of solids without dissolution. 

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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. 

C. W. Magee. Critical Parameters Affecting Precision and Accuracy in Spark Source Mass Spectrometry with Electrical Detection. PhD thesis, Univetsity of Virginia, University Microfilms, Ann Arbot, MI, 1973. 

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-... 

Spark Source Mass Spectrometry Spark Source Mass Spectrometry... 

H. Kramer, S. Semel J.E. Abel, Trace Elemental Survey Analysis of Trinitrotoluene , PATR 4767 (1975) (An evaluation of the applicability of spark source mass spectrometry and thermal neutron activation for the detn of origin-related trace elemental impurities in TNT) 10) C. Ribando J. Haber-man, Origin-Identification of Explosives Via Their Composite Impurity Profiles I. The... 

Neutron Activation Analysis X-Ray Fluorescence Particle-Induced X-Ray Emission Particle-Induced Nuclear Reaction Analysis Rutherford Backscattering Spectrometry Spark Source Mass Spectrometry Glow Discharge Mass Spectrometry Electron Microprobe Analysis Laser Microprobe Analysis Secondary Ion Mass Analysis Micro-PIXE... 

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. 

Table 5.6 compares the ICP-AES results with data generated for the same sample by two other independent methods - isotope dilution spark source mass spectrometry (IDSSMS), and graphite furnace atomic absorption spectrometry (GFAAS). The IDSSMS method also uses 25-fold preconcentration of the metals and matrix separation using the ion exchange procedure, following isotope... 

Precision expressed as 95% confidence intervals Spark source mass spectrometry, internal standard method From [735]... 

Heavy Metals, Isotope Dilution, Spark Source Mass Spectrometry, and Inductively Coupled Plasma Atomic Emission Spectrometry... 

A logical approach which serves to minimise such uncertainties is the use of a number of distinctly different analytical methods for the determination of each analyte wherein none of the methods would be expected to suffer identical interferences. In this manner, any correspondence observed between the results of different methods implies that a reliable estimate of the true value for the analyte concentration in the sample has been obtained. To this end Sturgeon et al. [21] carried out the analysis of coastal seawater for the above elements using isotope dilution spark source mass spectrometry. GFA-AS, and ICP-ES following trace metal separation-preconcentration (using ion exchange and chelation-solvent extraction), and direct analysis by GFA-AS. These workers discuss analytical advantages inherent in such an approach. 

Identification and structural analysis of organic compounds. Determination of trace impurities in a wide range of inorganic materials (spark source mass spectrometry). 

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. 

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) ... 

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