Spectrophotometry infrared

Infrared spectrophotometry is a familiar established analytical technique which provides identification of compounds by fingerprint spectra, of which a vast library is available. Both liquid and gaseous samples may be easily analysed and therefore modifications of established sample handling techniques have enabled both GC and HPLC instruments to be readily interfaced. Ideally, scan times of less than 1 s are required to be able to record each peak and peak shoulders. Instrument sensitivity is sufficient so that on the fly recording of spectra can be obtained from GC and HPLC eluants which contain nanograms of sample per ml mobile phase, for example, 10 ng sample in 100 pi GC-IR sample cell. Fourier transform infrared (FTIR) instruments are able to meet these criteria but until recently the instrumentation and computer system have been too expensive for routine use. The new generation of 

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Generally, cmde sulfur contains small percentages of carbonaceous matter. The amount of this impurity is usually determined by combustion, which requires an exacting technique. The carbonaceous matter is oxidized to carbon dioxide and water the carbon dioxide is subsequently absorbed (18). Automated, on-stream determination of impurities in molten sulfur has been accompHshed by infrared spectrophotometry (35). 

Determination. Various classical techniques are used for the analysis of vanillin, including colorimetric, gravimetric, spectrophotometric, and chromatographic (tic, gc, and hplc) methods. The Food Chemical s Codex (FCC) prescribes infrared spectrophotometry for identifying and testing vanillin. However, more vanillin analyses are made by either gc or hplc. 

Infrared Spectrophotometry. The isotope effect on the vibrational spectmm of D2O makes infrared spectrophotometry the method of choice for deuterium analysis. It is as rapid as mass spectrometry, does not suffer from memory effects, and requites less expensive laboratory equipment. Measurement at either the O—H fundamental vibration at 2.94 p.m (O—H) or 3.82 p.m (O—D) can be used. This method is equally appticable to low concentrations of D2O in H2O, or the reverse (86,87). Absorption in the near infrared can also be used (88,89) and this procedure is particularly useful (see Infrared and raman spectroscopy Spectroscopy). The D/H ratio in the nonexchangeable positions in organic compounds can be determined by a combination of exchange and spectrophotometric methods (90). 

The quantitative phenylation of pyridine has been studied by two groups of workers. Dannley and Gregg showed that 2-, 3-, and 4-phenylpyridine are formed in relative amounts 58 28 14 in the phenylation of pyridine with dibenzoyl peroxide, as estimated by infrared spectrophotometry. Hey and his co-workers obtained the ratios shown in Table I for the phenylation of pyridine using four different sources of phenyl radicals. ... 

Optical methods of analysis are dependent either upon (i) measurement of the amount of radiant energy of a particular wavelength absorbed by the sample, or (ii) the emission of radiant energy and measurement of the amount of energy of a particular wavelength emitted. Absorption methods are usually classified according to the wavelength involved as (a) visible spectrophotometry (colorimetry), (b) ultraviolet spectrophotometry, and (e) infrared spectrophotometry. 

All infrared spectrophotometers are provided with chart recorders which will present the complete infrared spectrum on a single continuous sheet, usually with wavelength and wavenumber scales shown for the abscissa and with absorbance and percentage transmittance as the ordinates. More advanced instruments also possess visual display units on which the spectra can be displayed as they are recorded and on which they can be compared with earlier spectra previously obtained or with spectra drawn from an extensive library held in a computer memory. These modern developments have all led to quantitative infrared spectrophotometry being a much more viable and useful analytical procedure than it was just a few years ago. 

THE BEER-LAMBERT RELATIONSHIP IN QUANTITATIVE INFRARED SPECTROPHOTOMETRY... 

It has taken a long time for quantitative infrared spectrophotometry to become a commonly used procedure for several reasons. 

A F Fell and G Smith, Higher derivative methods in ultraviolet, visible and infrared spectrophotometry, Anal. Proc., 1982, 19, 28... 

Infrared spectra - continued origins and regions of, 741 Infrared spectrophotometry 741... 

The Beer-Lambert relationship in quantitative infrared spectrophotometry 752... 

Maris, M.A., C.W. Brown, GJ. Kavamos, "Nonlinear Multicomponent Analysis by Infrared Spectrophotometry", Anal. Chem. 1983 (55) 1694-1703. 

The development and adaptation of procedures for the separation, isolation, purification, identification, and analysis of the components of the pyrethrum mixture have been studied and evaluated. Results of studies to determine the molar extinction coefficient of pyrethrin I as well as a gas chromatographic procedure for the determination of pyrethrins are reported. The use of chromatographic separation procedures (including partition, adsorption, gas, and thin-layer chromatography), colorimetry, and infrared spectrophotometry are discussed. 

Reference substances can be used for confirmation of identity of the substance by, e.g. infrared spectrophotometry where the spectrum of the substance to be examined must be concordant with the spectrum of the GRS, or by thin layer chromatography where the migration and appearance of the spots of both the substance to be examined and the GRS are the same, or by liquid chromatography where the retention time of both the substance to be examined and the GRS are the same. 

When the monograph requires the identification of a substance by infrared spectrophotometry, comparison can be made to a reference spectrum. 

A mass-isotope dilution method for determining the gamma isomer of benzene hexachloride, in which gamma-hexadeuterobenzene hexachloride is used as a tracer molecule and the dilution is determined by use of infrared spectrophotometry, has been developed by Trenner et al. (52). Impurities have no effect on the accuracy of this method. 

Chemical Testing. Adequate instrumentation for a variety of different test methods should be available. Most stability-indicating chemical assays are performed by high-performance liquid chromatography. Occasionally, gas chromatography, infrared spectrophotometry, or spectrofluorimetry are used. Test... 

The fatty acids measured by these techniques have all been small monomeric molecules. Lamar and Goerlitz [ 125] studied the acidic materials in highly coloured water and found that most of the nonvolatile material was composed of polymeric hydroxy carboxylic acids, with some aromatic and olefinic unsaturation. Their methods included gas, paper, and column chromatography with infrared spectrophotometry as the major technique used for the actual characterisation of the compounds. 

Groups of ten male Crl CD rats were exposed to HCN in polymethymethacrylate exposure chambers under flow-through conditions (E.I. du Pont de Nemours 1981). The chamber atmosphere was measured continuously by infrared spectrophotometry measurements were validated by gas chromatography. The experiment was performed in duplicate with one set of animals exposed head-only to the test gas while the other set was allowed free movement inside the exposure chamber. Free-moving rats inhaled concentrations of 273 to 508 ppm for 5 min, 110 to 403 ppm for 15 min, 128 to 306 ppm for 30 min, or 76 to 222 ppm for 60 min. The postexposure observation period was 14 d, during which body weights were monitored. 

Data adequacy The study was well conducted. The HCN concentrations were continuously monitored using infrared spectrophotometry and validated by gas chromatography. 

Technician Velma Montoya, of the Actinide Analytical Chemistry Group at Los Alamos, works in a silica-free glove box to determine silicon content in plutonium samples using visible (near infrared) spectrophotometry. 

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