The aim of this study was to determine the pentosan content in pulps by a dual-wavelength spectrophotometric method. The method was based on the boiling reaction between pentosan and 12% hydrochloric acid, in which pentosan was subsequently converted to furfural. The concentration of furfural in the distillate was determined by the absorbance at 280 nm and 290 nm. Several different simultaneous equations were solved to obtain the concentrations of furfural in the distillate. The results showed that the method had an excellent accuracy (RSD ≤ 0.61%) and reproducibility (RSD = 3.25%). The spectral interference of the 5-hydroxymethyl-2-furaldehyde in the distillate was eliminated by the dual-wavelength measurement technique. Compared with the TAPPI method (colorimetric method), this method is simple, user-friendly, and practical and has high detection sensitivity.