The surface and structural change of human hair fibre have been analysed to determine the oxidation effects for bleached hairs. Three types of bleached hairs (6% H2O2 bleach, 9% H2O2 commercial bleach and commercial persulphate bleach (contains 9% H2O2)) as well as virgin hair were evaluated with the increasing treatment time using Scanning Electron Microscopy (SEM), Reflective Spectrophotometry, Differential Scanning Calorimetry (DSC) and Fourier Transform Infrared (FTIR) Spectroscopy. It is obvious that longer treatment times result in the greater surface and structural damage. However, commercial persulphate bleach causes less surface damage for the cuticle. 6% H202 bleach has overall moderate damage effects on both cuticle and cortex over the treatment time. 9% H2O2 commercial bleach indicates two different damage stages. The first 1.5h bleached hairs show mild oxidation to the surface, whereas the damage becomes heavy after 2h. This phenomenon results in that 9% H2O2 commercial bleach has a more intensive oxidation damage in the cortex than the commercial persulphate bleach. This is in line with DSC investigation which shows that the intermediate filament of 9% H2O2 commercial bleach is heavily damaged after the extensive oxidation time (greater than or equal to2h). Although commercial persulphate bleach contains the stronger oxidising agent, it has a less surface damage than 9% H2O2 commercial bleached hair in FTIR-ATR measurement, and a similar oxidation effect on the matrix as 6% H202 bleached hair in FTIR transmission investigation. In addition, it has been verified by colour measurements that bleached hairs have an overall lighter, yellowish and reddish colour. Consequently, commercial persulphate bleached hair is much lighter and more yellow than 9% H2O2 commercial bleached hair and 6% H202 bleached hair. DSC investigations reveal that the three bleaches have a homogenous oxidation effect on IFs and IFAPs. The deconvolution results using three Gaussian distributions confirm this observation. The stronger bleach results in a homogenous structural damage on both para- and ortho-cortex with increasing bleaching time. Commercial persulphate bleach and 9% H2O2 commercial bleach have a progressive damage effect on the ortho- and para- cortex than 6% H202 bleach. Kinetics analysis is conducted for the virgin and bleached hairs by using various heating rates according to ASTM-E698. The activation energies of 260 kJ/mol for the virgin hair and 295 kJ/mol for the commercial persulphate bleached hair (2h) are determined from the slope of the regression line of peak temperature, TD (as 1/TD) and heating rate, β (as lnβ) on the basis of the Arrhenius-equation. The predominant structural damage for various heating rates only occurs in the IF. It is shown that a linear increase in DeltaHD occurs for lower heating rates, while it is constant for higher heating rates. This can be ascribed to the hypothesis that a lower heating rate favours a crystal transformation change (alpha-β transformation), while a higher rate favours a crystalline-amorphous transformation. SEM examines the morphological changes of hair samples after DSC. The cortex has been dissolved at the lower heating rate. The commercial persulphate bleached hairs (2h) show an overall shrunk cuticle surface and fewer and smaller hydrolysed protein granules, due to the previous damage of the alpha-helix in the cortical cell.