Using a coupling process of neutralization-nanofiltration-crystallization, pure ammonium metatungstate (AMT) was prepared. The effects of chemical neutralization of ammonium paratungstate (APT) by nitric acid, operating pressure, AMT concentration, the volume of washing water on the coupling process were systematically discussed. It was found that the better conditions of AMT preparation were as follows: the neutralization temperature was 80-95 degreesC, pH value was 2.0-3.5; the operating pressure of HDS-12-2 nanofiltration was 1.5-2.0 MPa, the density of AMT crystallization solution was 2.39 kg/L, and then cooling. APT conversion efficiency (8) to AMT was more than 97.62%. The removal ratio of nitrate ion (NO3-) was more than 99% while AMT rejection (R-AMT) was 99.9%. Besides, small-grained, even-proportioned, white-colored and high-purified AMT crystal was be obtained and analyzed. This method has several advantages such as simple technological process, short production cycle. lower environmental pollution and high quality. (C) 2004 Elsevier B.V. All rights reserved.