Simple spectrum, from solid sample

In this experiment, tritiated water is purified by simple distillation, and the tritium beta particles in the condensate are measured with a liquid scintillation (LS) counter. Such distillation also can collect tritiated water samples from solids. Tritium in other forms must be processed before it can be counted like tritium in water for example, tritiated hydrogen gas and tritiated organic substances can be oxidized to form water. Additional separations may be needed if the liquid or solid sample contains radioactive gases or volatile substances other than tritium that may be collected with the distilled tritiated water. Such radioactive impurities can be identified in the data output from the LS counter of an energy spectrum that differs from that of pure tritium, or of counts in energy regions where tritium counts are not found. 

Solid samples may be heated and vaporized using laser energy with the additional benefit that compounds may be ionized with the same laser, all at ambient pressure, and characterized in an IMS drift tube. While lasers were used with mobility spectrometers initially for selective photoionization of vapors only,° ° ions were observed from laser contact with solids, including metals and salts. This was not simple vaporization by heating and instead was understood as ablation and ionization. In laser desorption ionization (LDI), the laser pulse initiates a mobility spectrum with a... 

Level 1 sampling provides a single set of samples acquired to represent the average composition of each stream. This sample set is separated, either in the field or in the laboratory, into solid, liquid, and gas-phase components. Each fraction is evaluated with survey techniques which define its basic physical, chemical, and biological characteristics. The survey methods selected are compatible with a very broad spectrum of materials and have sufficient sensitivity to ensure a high probability of detecting environmental problems. Analytical techniques and instrumentation have been kept as simple as possible in order to provide an effective level of information at minimum cost. Each individual piece of data developed adds a relevant point to the overall evaluation. Conversely, since the information from a given analysis is limited, all the tests must be performed to provide a valid assessment of the sample. 

Laser ablation can be carried out on any material without special sample preparation. The laser beam can be directed onto a defined spot of the sample or moved to different parts to analyse over a defined area. It can be moved in an XYZ plane using a stepper motor and driven in translational motions on which the cell is mounted and with more expensive models can be turned for analysis in other parts of the sample. Lasers can operate in UV, visible, and IR regions of the spectrum and a recent development in laser technology uses neodymium yttrium aluminium garnet (Nd YAG) which gives high repetition rate at a comparatively low power. This method of analysis is suited to bulk analysis of solid materials and the amount of volatility varies from sample to sample. The size of the laser spot can vary from 10 to 250 pm and little or no sample preparation is required. Errors are greatly reduced because of the simple sample preparation, and the fact that no solvents are required reduces interferences. 

Because no separation is used, only crude information about the purity of the compounds can be obtained. For example, if unreacted, synthetic starting materials (Fig. 10b) are present in a sample of a combinatorial product (Fig. 10a), these can show up in the mass spectrum of the crude product (Fig. 10c). Because the starting materials are often structurally different from the finished product, a simple extraction can be used after the synthesis to remove much of the unused reactants and obtain a cleaner mass spectrum (Fig. lOd) for a solution-phase product. Conversely, washing the resin after solid-phase synthesis or using a scavenger resin in a solution-phase synthesis can also yield improved purity by removing these excess reactants. When direct flow injection is used to characterize combinatorial libraries, it is best to avoid dimethyl sulfoxide (DMSO) as a solvent, because it interferes with reliable ionization of the analytes. 

A simple example of how a filter is used is shown in Fig. 8.16. The solid line spectrum is the output of a Rh tube operated at 20 kV with no filter between the tube and the detector. The Rh L line at 2.69 keV is seen, along with a broad continuum of X-rays from 4 to 19 keV. If the Rh L line gets scattered into the detector, as it can from a crystalhne sample, it can be mistaken for an element in the sample or may overlap another line, causing spectral interference. Placing a cellulose filter over the tube window causes the low energy Rh characteristic line to be absorbed only the continuum radiation reaches the detector, as shown by the dotted line spectmm. 

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