The toxicity of beryllium and aluminium as well as the need for sensitive and selective methods for determining these elements are well documented. Several instrumental methods for determination of beryllium and aluminium by spectrophotometry, 1-3 spectrofluorimetry, 4-7 flame atomic absorption spectrometry (AAS), 8 graphite furnace atomic absorption spectrometry (GFAAS), 9 and inductively coupled plasma atomic emission spectrometry (ICP-AES) 10 have been reported. The complexes of Be(II) and Al(III) with Chrome Azurol S (CAS) have been proposed for the spectrophotometric determination of both the elements individually. 11,12 Simultaneous determination of Al(III) and Be(II) was also reported. [13][14][15] Capitán et al. 13 determined Al(III) and Be(II) in mixtures in the range of 0.5 -5.0 ng mL -1 for both the cations, by first-derivative synchronous solid-phase spectrofluorometry, based on their complexes with morine.A derivative spectrophotometric method for simultaneous determination of Al(III) and Be(II) in the ranges of 108.0 -1080.0 ng mL -1 and 36.0 -360.0 ng mL -1 , respectively, was reported based on their complexes with 5,8-dihydroxy-1,4-naphthoquinone. 14 Valencia et al. 15 reported a method for simultaneous determination of Al(III) and Be(II) by first derivative solid phase spectrophotometric method based on their complexes with Eriochrome Cyanine R. The application range was up to 60 ng mL -1 for aluminium and up to 4.0 ng mL -1 for beryllium.H-point standard addition method (HPSAM) is a suitable method for resolving mixtures of substances with overlapping spectra. [16][17][18][19][20] The greatest advantage of HPSAM is that it can remove the errors resulting from the presence of an interference and reagent blank. 16 HPSAM can determine the two components simultaneously with extensively or even coincident overlapping spectra. 18 The Bosch-Reig et al. 21 method was aimed at establishing the fundamentals for application of the HPSAM to kinetic data for the simultaneous analysis of binary mixtures or the calculation of analyte concentrations completely free from bias error. For this purpose, they used two variants of the HPSAM: one is applied when the reaction of one component is faster than that of the other or the latter does not take place at all. This variant of the method is based on the assumption that only analyte X evolves with time and that the other species or interferents do not affect the analytical signal with time. In this case the variables to be fixed are two times t1 and t2 at which the species Y, which does not evolve with time or over the range between these times, should have the same absorbance. The other variant of the method is used when the rate constants of the two components are time-dependent. In this case, the two species in a mixture, X and Y, both evolve with time.In this paper, we describe a rapid, simple, precise and accurate method for the simultaneous determination of beryllium and aluminium by spectrophotometric H-point standard addition method. This method is based o...