This article presents the development of an automatic on-line measurement system for characterizing a nanoparticle manufacturing process known as Arc Spray Nanoparticle Synthesis System (ASNSS). The ASNSS has been developed to generate metal nanoparticles and to explore the optimum system parameters for producing the desired nanopowders. Preliminary experimental results indicate that the size of nanoparticles, widely ranging from 10nm to 300nm, is significantly affected by the process parameters such as operating pressure, temperature, electrical current and type of dielectric liquid used. The on-line measurement system was developed to provide an effective multi-solution for characterizing the nanoparticle synthesis process and for monitoring the manufacturing quality of the ASNSS. Experiments were conducted to identify the optimum sampling period and volume of the particle suspension for accurate sampling and data acquisition. Experimental results revealed that a sampling duration of 20 minutes and a dielectric volume of 40 c.c. can achieve effective data representation while maximizing the sampling efficiency.