The invention discloses a method for preparing a glow discharge mass spectrometer analysis test sample. The method comprises the following steps: a) putting refractory metal powder to be analyzed into a graphite mold which is internally coated with a demolding agent; b) forming the powder by using a pressure sintering method; c) milling a formed blank. By using the method disclosed by the invention, the test sample is relatively high in compactness and is clean in surface while the content of impurities in the sample is kept unchanged as much as possible, so that the accuracy and the precision of the glow discharge mass spectrum analysis result are ensured, and meanwhile the test sample prepared by using the method has the advantages of high analysis speed and high efficiency.