Analysis reaction

This overview covers the major teclnhques used in materials analysis with MeV ion beams Rutherford backscattering, chaimelling, resonance scattering, forward recoil scattering, PIXE and microbeams. We have not covered nuclear reaction analysis (NRA), because it applies to special incident-ion-target-atom combinations and is a topic of its own [1, 2]. 

The automated amino acid analy2er depends on ion-exchange chromatography (117) and is now a routine tool for the analysis of amino acid mixtures (118). This most advanced machine can detect as Htde as 10 pmol in ninhydrin reaction analysis. One-half to two hours are required for each analysis. An analysis chart is shown in Figure 2. 

Petersen, Chemical Reaction Analysis, Prentice-Hall, 1965. 

Petersen, E. E. 1965, Chemical Reaction Analysis. Prentice-Hall, Inc., Englewood Cliffs, NJ.. 

All the techniques discussed here involve the atomic nucleus. Three use neutrons, generated either in nuclear reactors or very high energy proton ajccelerators (spallation sources), as the probe beam. They are Neutron Diffraction, Neutron Reflectivity, NR, and Neutron Activation Analysis, NAA. The fourth. Nuclear Reaction Analysis, NRA, uses charged particles from an ion accelerator to produce nuclear reactions. The nature and energy of the resulting products identify the atoms present. Since NRA is performed in RBS apparatus, it could have been included in Chapter 9. We include it here instead because nuclear reactions are involved. 

Nuclear reaction analysis (NRA) is used to determine the concentration and depth distribution of light elements in the near sur ce (the first few lm) of solids. Because this method relies on nuclear reactions, it is insensitive to solid state matrix effects. Hence, it is easily made quantitative without reference to standard samples. NRA is isotope specific, making it ideal for isotopic tracer experiments. This characteristic also makes NRA less vulnerable than some other methods to interference effects that may overwhelm signals from low abundance elements. In addition, measurements are rapid and nondestructive. 

Figure 7 Lateral profiles of carbon and lithium measured by nuclear reaction analysis.

W. K. Chu, J. W. Mayer, and M. -A. Nicolet. Backscattering Spectrometry. Academic Press, New York, 1978, brief section on nuclear reaction analysis, discussions on energy loss of ions in materials, energy resolution, surface barrier detectors, and accelerators also applicable to NRA ... 

Metastable quenching spectroscopy Nuclear Reaction Analysis Rutherford back-scattering spectroscopy (or HEIS high-energy ion scattering)... 

The overall rate of a chain process is determined by the rates of initiation, propagation, and termination reactions. Analysis of the kinetics of chain reactions normally depends on application of the steady-state approximation (see Section 4.2) to the radical intermediates. Such intermediates are highly reactive, and their concentrations are low and nearly constant throughout the course of the reaction ... 

Fig. 5. Hydrogen depth profile of a deuterated polystyrene PS(D) film deposited on a protonated polystyrene PS(H) film on top of a silicon wafer as obtained by l5N-nuclear reaction analysis ( 5N-NRA). The small hydrogen peak at the surface is due to contamination (probably water) of the surface. The sharp interface between PS(D) and PS(H) is smeared by the experimental resolution (approx. 10 nm at a depth of 80 nm) [57], The solid line is a guide for the eye...

Froment, G. F. and Bischoff, K B., Chemical Reaction Analysis and Design, 2nd ed., Wiley, New York, 1990. 

Addition of, say, a C02Et group would allow Diels-Alder disconnection leading eventually to cycloheptanone. A better strategy is to add a carbonyl group to make an enone (31) with Robinson annelatlon as the key reaction. Analysis... 

Doraiswamy, L. K., Sharma, M. M., Heterogeneous reactions - analysis, examples and reactor design, Wiley -Interscience Publications, New York (1984). 

Andraos, J. (2005) Unification ofReaction Metrics for Green Chemistry Applications to Reaction Analysis. Organic Process Research and Development, 9, 149-163. 

Doraiswamy, L.K. and Sharma, M.M., 1984, Heterogeneous Reactions Analysis, Examples and Reactor Design , Vol. 2, Wiley-interscience, New York. 

The parameter p (= 7(5 ) in gas-liquid sy.stems plays the same role as V/Aex in catalytic reactions. This parameter amounts to 10-40 for a gas and liquid in film contact, and increases to lO -lO" for gas bubbles dispersed in a liquid. If the Hatta number (see section 5.4.3) is low (below I) this indicates a slow reaction, and high values of p (e.g. bubble columns) should be chosen. For instantaneous reactions Ha > 100, enhancement factor E = 10-50) a low p should be selected with a high degree of gas-phase turbulence. The sulphonation of aromatics with gaseous SO3 is an instantaneous reaction and is controlled by gas-phase mass transfer. In commercial thin-film sulphonators, the liquid reactant flows down as a thin film (low p) in contact with a highly turbulent gas stream (high ka). A thin-film reactor was chosen instead of a liquid droplet system due to the desire to remove heat generated in the liquid phase as a result of the exothermic reaction. Similar considerations are valid for liquid-liquid systems. Sometimes, practical considerations prevail over the decisions dictated from a transport-reaction analysis. Corrosive liquids should always be in the dispersed phase to reduce contact with the reactor walls. Hazardous liquids are usually dispensed to reduce their hold-up, i.e. their inventory inside the reactor. 

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... 

Cortright RD, Dumesic JA. 2001. Kinetics of heterogeneous catal)4ic reactions analysis of reaction schemes. Adv Catal 46 161 -264. 

ReactIR refers to the real time, in situ monitoring of the IR spectrum of the reaction mixture with a ReactIR 4000 Reaction Analysis System available from AS I Applied Systems. 

---