Beam, reference cell

In these instruments the monochromated beam of radiation, from tungsten and deuterium lamp sources, is divided into two identical beams, one of which passes through the reference cell and the other through the sample cell. The signal for the absorption of the contents of the reference cell is automatically subtracted from that from the sample cell giving a net signal corresponding to the absorption for the components in the sample solution. 

The differential refractometer monitors the deflection of a light beam caused by the difference in refractive index between the contents of the sample cell and those of the reference cell. A beam of light from an... 

Characterization of the reaction intermediate is facilitated by studies in a flow system in which the sample cell and a reference cell are mounted in series in a double beam spectrometer (IS). Not only can we observe the intermediate bands under rigorous steady state conditions, but we can monitor the conversion by sampling the effluent. In addition, the reference cell assures the spectrum we see is that of surface species. Primitive analysis of the kinetics reveals the intermediate is favored by relatively high ethylene pressures hence, use of a reference cell to cancel contributions of the gas phase is an important factor. 

Like much instrumentation working in the IR/visible/UV region of the spectrum, most modern UV/visible spectrometers are of the dual-beam type, since this eliminates fluctuations in the radiation source. The principle of this has been described in detail in Section 3.2. Radiation from the source is split into two by a beam splitter, and one beam is passed through the sample cell (as in a single beam instrument). The other beam passes through a reference cell, which is identical to the sample cell, but contains none of the analyte... 

This is usually an electrically heated filament whose rays are separated by hollow mirrors into two beams, one for sample and the other for reference cell. 

The beam chopper forces radiation to come alternately from the sample and the reference cell. 

A thermocouple as radiation detector converts the alternating IR beams from the sample and reference cell into an alternating electric current. 

In practice, double-beam instruments are used where the absorption of a reference cell, containing only solvent, is subtracted from the absorption of the sample cell. Double beam instruments also cancel out absorption due to the atmosphere in the optical path as well as the solvent. 

The operation of a commercial recording IR spectrometer (Fig. 6.5) is as follows. The source radiation is reflected from two mirrors to give two identical beams one beam passes through the sample cell, the other through an empty reference cell (if the sample is in solution, the reference cell is filled with the solvent). A chopper system then causes alternately the... 

Figure 6. Instrumental schematic for vacuum UV photofragmentation-laser induced fluorescence measurement of ammonia SHGC, second harmonic generation crystal SFMC, sum frequency mixing crystal BS, beam splitter BD, beam dump TP, turning prism CL, cylindrical lens R, reflector TD, trigger diode OSC, oscillator cell AMP, amplifier cell BE, beam expander G, grating OC, output coupler M, mirror BC, beam combiner L, lens A, aperture PD, photodiode SC, sample cell RC, reference cell FP, filter pack SAM.PMT, sample cell photomultiplier REF.PMT, reference cell photomultiplier PP, additional photomultiplier port EX, exhaust and CGI, calibration gas inlet to flow line. (Reproduced with permission from reference 15. Copyright 1990 Optical Society of America.)...

Because most FT—IR spectrometers have a computerized data system as an integral component of the instrument, it is a relatively simple matter for programs to be written that operate on spectra as soon as they have been computed from the interferogram. One of the most important of these programs is the scaled absorbance subtraction routine. This program can be used to achieve the same result as placing a sample in the reference beam of the spectrometer, but the thickness of the reference cell or sample does not need to be controlled as accurately... 

Two UV detectors are also available from Laboratory Data Control, the UV Monitor and the Duo Monitor. The UV Monitor (Fig.3.45) consists of an optical unit anda control unit. The optical unit contains the UV source (low-pressure mercury lamp), sample, reference cells and photodetector. The control unit is connected by cable to the optical unit and may be located at a distance of up to 25 ft. The dual quartz flow cells (path-length, 10 mm diameter, 1 mm) each have a capacity of 8 (i 1. Double-beam linear-absorbance measurements may be made at either 254 nm or 280 nm. The absorbance ranges vary from 0.01 to 0.64 optical density units full scale (ODFS). The minimum detectable absorbance (equivalent to the noise) is 0.001 optical density units (OD). The drift of the photometer is usually less than 0.002 OD/h. With this system, it is possible to monitor continuously and quantitatively the absorbance at 254 or 280 nm of one liquid stream or the differential absorbance between two streams. The absorbance readout is linear and is directly related to the concentration in accordance with Beer s law. In the 280 nm mode, the 254-nm light is converted by a phosphor into a band with a maximum at 280 nm. This light is then passed to a photodetector which is sensitized for a response at 280 nm. The Duo Monitor (Fig.3.46) is a dual-wavelength continuous-flow detector with which effluents can be monitored simultaneously at 254 nm and 280 nm. The system consists of two modules, and the principle of operation is based on a modification of the 280-nm conversion kit for the UV Monitor. Light of 254-nm wavelength from a low-pressure mercury lamp is partially converted by the phosphor into a band at 280 nm. 

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