Abstract: One important parameter of single wall carbon nanotubes (SWCNTs) to be measured is chiral index. Chiral indices not only contain information about diameter and chiral angle, but also indicate electronic properties of SWCNTs. Generally, near infrared photoluminescence fluorescence spectrometer is a widely used method for chiral indices identification. However, there is no standard calibration procedures for this kind of fluorescence spectrometer, resulting in a lack of comparability between the results measured by various instruments. Based on this kind of fluorescence spectrometer, the principle and configuration of fluorescence spectrometer were briefly introduced, and the calibration procedures were discussed including excitation light path calibration and emission light path calibration.The method was to calibrate the excitation wavelength and emission wavelength to the 467 nm and 1 053 nm using standard xenon lamp spectrum and standard laser glass spectrum respectively. After calibration, chiral indices of SWCNTs were measured using calibrated instrument and ultraviolet-visible-near infrared spectrometer, and the results both are (11, 1)，(8, 7)，(10, 3)，(9,5)，(11, 3)，(8, 6)，(9,2)，(7, 6)，(8, 4)，(7, 5)，(10,2). The comparison results indicate that the calibration procedures are accurate.