Microwave monitoring techniques

It is common to employ microwave power monitoring by means of a dual-directional coupler in the waveguide transmission system between the power tube and the useful load. Part of the coupled signals may be used for examination with spectmm analy2ers, frequency meters, and other microwave instmmentation for special purposes. Generally, this is not necessary in a practical appHcation. Many microwave measurement techniques have been described (59,60). AvailabiHty of components, plumbing, and instmmentation is weU described in trade journals. 

KDC Technology has developed a cost-effective microwave sensor technique for monitoring constituents and moisture in a wide variety of products including foods (KDC 1993). The KDC sensor is adaptable to measurement of process parameters of products contained in tubes, chutes, bins, vessels as well as moving on conveyer lines. 

A microwave attenuation technique was used to monitor in-situ oil/water saturations during enhanced recovery for each alkaline core flood. 

The carrier decay can also be monitored directly without the need for contacts. Contactless measurements are very desirable because they are fast and non-destructive. For example, a wafer can be pulled from the process cycle, measured and then re-inserted into the process. One method of PCD contactless measurements is the microwave reflection technique. [74] Excess carriers are created by light pulses as in the conventional PCD method. The time-dependent photoconductivity is monitored by detecting the time-dependent microwave reflection from the sample s surface. 

Microwave Hall experiments have been performed in our laboratory.16 They have shown that the mobility of charge carriers in semiconductors can be measured quite reliably even if the semiconductors are only available in the form of a powder. The measurement technique itself is relatively complicated and involves, for example, rectangular waveguides, which can be rotated against each other on opposite sides of the sample to monitor the phase rotation. In the two-mode resonator, two modes of... 

Abstract Current microwave-assisted protocols for reaction on solid-phase and soluble supports are critically reviewed. The compatibility of commercially available polymer supports with the relatively harsh conditions of microwave heating and the possibilities for reaction monitoring are discussed. Instrmnentation available for microwave-assisted solid-phase chemistry is presented. This review also summarizes the recent applications of controlled microwave heating to sohd-phase and SPOT-chemistry, as well as to synthesis on soluble polymers, fluorous phases and functional ionic liquid supports. The presented examples indicate that the combination of microwave dielectric heating with solid- or soluble-polymer supported chemistry techniques provides significant enhancements both at the level of reaction rate and ease of purification compared to conventional procedures. 

PEG polymers are widely used as water soluble supports [99]. Although these polymers suffer from easy loss of PEG oligomers, they are frequently used for the preparation of small organic molecules [100-105] and biopolymers [106,107]. The main benefit of PEG supports is their solubility in water as well as most organic solvents. Also, as opposed to most solid-phase techniques, PEG polymers allow for easy on-bead NMR monitoring. Soluble PEG supports have been used frequently in synthetic microwave chemistry protocols [108-122]. 

The basic features of an epr spectrometer are shown in Figure 2.95. The microwave source is a Klystron tube that emits radiation of frequency determined by the voltage across the tube. Magnetic fields of 0.1 — 1 T can be routinely obtained without complicated equipment and are generated by an electromagnet. The field is usually modulated at a frequency of 100kHz and the corresponding in-phase component of the absorption monitored via a phase-sensitive lock-in detector. This minimises noise and enhances the sensitivity of the technique. It is responsible for the distinctive derivative nature of epr spectra. Thus, the spectrum is obtained as a plot of dA/dB vs. 

Buschmuller et have demonstrated that microwave resonance can be used effectively as means to monitor the moisture levels in a fluidized-bed dryer during the granulation process. The penetration depth of microwave resonance may be limited to a few microns, and hence this technique may not have any real advantages over NIR which has also been used for monitoring moisture in dryers, and has the advantage of providing chemical information such as solvent levels in addition to water, and other important properties such as polymorphic form, and particle size. 

ESEEM is a pulsed EPR technique which is complementary to both conventional EPR and ENDOR spectroscopy(74.75). In the ESEEM experiment, one selects a field (effective g value) in the EPR spectrum and through a sequence of microwave pulses generates a spin echo whose intensity is monitored as a function of the delay time between the pulses. This resulting echo envelope decay pattern is amplitude modulated due to the magnetic interaction of nuclear spins that are coupled to the electron spin. Cosine Fourier transformation of this envelope yields an ENDOR-like spectrum from which nuclear hyperfine and quadrupole splittings can be determined. 

Phase Dynamics utilizes a unique, patented microwave concept to diagnose and measure molecular transformation process parameters with high sensitivity and accuracy (Phase Dynamics 1992). While originally developed for fluid measurements, the instrumentation is adaptable to most pumpable process lines and to some batch applications. The technique has been utilized for compositional analyses of true solutions as well as complex solid-liquid systems such as colloids and emulsions. Monitoring of molecular transitions which occur in cooking processes, hydrogenation, gelatinization and hydrolysis can also be monitored. 

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