A complete chromatographic analysis usually implies the identification and quantitative determination of the concentrations of all or only particular target components in test samples. To solve the latter problem, various quantitative methods of analysis are used; these differ in sample preparation and data processing techniques [1,2]. The most accurate versions of determination imply the availability of certified reference materials, which are required for the preparation of calibration mixtures (absolute calibration and external standard techniques); the direct addition to test samples (standard addition); or the predetermination of the calibration coefficients ( f i ) expt of the target components with reference to standard substances chosen (internal standard and internal normalization). In the absence of reference samples, quantitative analysis is usually restricted to the use of only external and internal standards or internal normalization on the condition that the chromatographic relative sensitivity coefficients ( f i ) calcd for various compounds were theoretically precalculated. In the presentation of analytical results obtained for chemically similar substances by the internal normalization method with the use of flame-ionization detectors (FIDs), it is often assumed that f i ≡ const. The same approach (the calculation of relative peak areas) is used in processing analytical results obtained by chromatography-mass spectrometry in multicomponent mixtures, although the ionization cross sections of various organic compounds are dramatically different [3].Two objective causes are responsible for such a reduction in the requirements imposed on the results of the quantitative determination of the composition of complex samples. First is the problem of finding analyte reference samples, long considered as insignificant and completely irrelevant to quantitative analysis. However, the attitude to this problem has changed in recent years because the inappropriately great consumption of time at this stage or the high cost of these samples can make unreasonable the performance of the analysis in general [4][5][6][7][8]. Second, various procedures for the theoretical evaluation of relative detector sensitivity coefficients to various compounds based on the composition (or, more rarely, the structure) of analytes [1, vol. 2, p. 173; 7] give only estimated values of ( f i ) calcd , usually without estimated errors; in particular, they do not reflect the known effects of analytical conditions on the values of ( f i ) expt .The effects of conditions (detector geometry, flame temperature, carrier gas, etc.) were characterized in the greatest detail for the absolute characteristics of FID sensitivity [1]. However, variations in the relative values ( f i ) expt were usually considered to be comparatively small, and they were ascribed to the random component of determination errors. For this reason, specific features of data processing by the internal normalization method were not related to the temperature conditions of...