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Experimental results of a diesel engine have shown that using split-injection can reduce the NOx and particulate emissions. For understanding the mechanism of emissions reduction, mixture formation in split-injection diesel sprays was characterized in the present paper. A dual-wavelength laser absorption-scattering (LAS) technique was developed by use of the second harmonic (532nm) and the fourth harmonic (266nm) of a pulsed Nd:YAG laser as the incident light and dimethylnaphthalene (DMN) as the test fuel. By applying this technique, imaging was made of DMN sprays injected into a high-temperature and high-pressure constant volume vessel by a single-hole nozzle incorporated in a common rail injection system for D.I. diesel engine. The line-of-sight optical thickness of both fuel vapor and droplets in the sprays was yielded from the sprays images.