Survey analysis

In the report analytieal figures of merit of ICP-MS and -AES teehniques in eombination with pre-eoneentration of traee elements for survey analysis of high purity metals and their oxides used as the preeursors for oxide monoerystals produetion will be presented and eompared to that of direet ICP-MS and -AES teehniques. 

Laser based mass spectrometric methods, such as laser ionization (LIMS) and laser ablation in combination with inductively coupled plasma mass spectrometry (LA-ICP-MS) are powerful analytical techniques for survey analysis of solid substances. To realize the analytical performances methods for the direct trace analysis of synthetic and natural crystals modification of a traditional analytical technique was necessary and suitable standard reference materials (SRM) were required. Recent developments allowed extending the range of analytical applications of LIMS and LA-ICP-MS will be presented and discussed. For example ... 

In Laser Ionization Mass Spectrometry (LIMS, also LAMMA, LAMMS, and LIMA), a vacuum-compatible solid sample is irradiated with short pulses ("10 ns) of ultraviolet laser light. The laser pulse vaporizes a microvolume of material, and a fraction of the vaporized species are ionized and accelerated into a time-of-flight mass spectrometer which measures the signal intensity of the mass-separated ions. The instrument acquires a complete mass spectrum, typically covering the range 0— 250 atomic mass units (amu), with each laser pulse. A survey analysis of the material is performed in this way. The relative intensities of the signals can be converted to concentrations with the use of appropriate standards, and quantitative or semi-quantitative analyses are possible with the use of such standards. 

SALI applies two methods of post-ionization, MPI and SPI, each of which can be used in one of the three modes of analysis survey analysis, depth profiling, and mapping ... 

Laser ionization mass spectrometry or laser microprobing (LIMS) is a microanalyt-ical technique used to rapidly characterize the elemental and, sometimes, molecular composition of materials. It is based on the ability of short high-power laser pulses (-10 ns) to produce ions from solids. The ions formed in these brief pulses are analyzed using a time-of-flight mass spectrometer. The quasi-simultaneous collection of all ion masses allows the survey analysis of unknown materials. The main applications of LIMS are in failure analysis, where chemical differences between a contaminated sample and a control need to be rapidly assessed. The ability to focus the laser beam to a diameter of approximately 1 mm permits the application of this technique to the characterization of small features, for example, in integrated circuits. The LIMS detection limits for many elements are close to 10 at/cm, which makes this technique considerably more sensitive than other survey microan-alytical techniques, such as Auger Electron Spectroscopy (AES) or Electron Probe Microanalysis (EPMA). Additionally, LIMS can be used to analyze insulating sam-... 

Most applications of LIMS are in failure analysis. A typical microanalytical failure analysis problem, for example, may involve determinating the cause of corrosion in a metallization line of an integrated circuit. One can achieve this by performing an elemental survey analysis of the corroded region. Since it is not always known which elements are normal constituents of the material in question and which are truly contaminants, the vast majority of these analyses are performed by comparing the elemental make-up of the defective region to that of a control region. The com-... 

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... 

The SSMS point-to-plane surface technique has been shown to be particularly useful in the survey analysis of epitaxial films, heavy metal implant contamination, diflRision furnace contamination, and deposited metal layers. 

Abel, Trace Elemental Survey Analysis of TNT , PATR 4257 (1975) 76) T.H. Maugh,... 

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... 

Allowance for direct mixture analysis (simple spectra) survey analysis... 

Trends in element analysis are multi-element (survey) analysis, lower concentration levels, micro/local element analysis and speciation (coupling with chromatography). An overview of the determination of elements in polymeric materials is available [7], Reviews on sample preparation for trace analysis are given in refs [8-10]. Quality assurance of analytical data in routine elemental analysis has been discussed [11], Organic analysis is obviously much more requested in relation to polymer/additive matrices than elemental analysis. 

Rapid survey analysis of solids, powders, composites, films, coatings, pastes, slurries and liquids... 

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... 

NIOSH. 1977j. National occupational hazard survey. Vol. Ill Survey analysis and supplemental tables. Cincinnati, OH U.S. Department of Health, Education, and Welfare. Public Health Service, Centers for Disease Control, National Institute for Occupational Safety and Health, Division of Surveillance, Hazard Evaluations, and Field Studies. DHEW (NIOSH) Publication No. 78-114, 346. 

Kalman DA. 1986. Survey analysis of volatile organics released from plastics under thermal stress. Am Ind... 

Miller HC, James RH, Dickson WR, et al. 1981. Evaluation of methodology for the survey analysis of solid wastes. ASTM Spec Tech PubI 760 240-266. 

The philosophy of a preliminary survey analysis is used to help define the extent of potential risk (Level I analysis). Data gathered in the Level I survey analysis is used as a protocol for more detailed analysis (Level II). At Level III, a detailed analysis is made as a function of system parameters and time. 

XPS is particularly suited to analyze solid materials in various materials science applications of polymeric materials. Several examples of the use of XPS to analyze the surface of solids in irregular forms such as fibers, powders, films, beads, and various extruded shapes such as o-rings will be presented. XPS can provide a rapid survey analysis as well as quantitative analysis within several percent depending on the sensitivity for the element in question. Unique structural information can often be obtained on solids that, due to their intractability and lack of solubility would present problems for investigation by other spectroscopic methods. 

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