Manufacturing Of Reference Material For Composition Analysis Of High Purity Molybdenum

A reference material for high-purity molybdenum composition analysis has been developed,which is suitable for the detection of solid samples by glow discharge mass spectrometry.The application of high purity molybdenum and analytical methods were investigated.The major analytical methods of trace impurities in high purity molybdenum are:ICP-AES,ICP-MS,ICP-MS,glow discharge mass spectrometry(GD-MS).Among this,GD-MS has the advantages of direct solid injection and low detection limit.It has gradually become a better method for the detection of trace impurities.However,them method needs to be corrected by matrix matching reference material.In this paper,ammonium molybdate was used as raw material and metal salt solution as doping reagent to develop the reference material for composition analysis of high-purity molybdenum.The preparation steps are as follows:composition design,liquid phase doping,agitation evaporation,hydrogenation reduction,mechanical agitation.The standard sample of molybdenum powder with particle size of 1-100 ?m was obtained.The homogeneity of the content of impurity elements in the sample was up to the standard through the F test.After sintering in hydrogen atmosphere,the samples of ? 20 × 8 mm molybdenum block were obtained.The changes of matrix morphology,impurity element content and homogeneity in the process of homogenization of standard samples were studied,and the law of impurity element loss in sintering process was explored.A batch of high-purity molybdenum quality control samples were prepared by pressing.The RSF of 7 elements such as Al,Fe,Cr,Co,Ni,Sb,Hf were corrected by using the intrinsic control samples for the detection of high-purity molybdenum samples by GD-MS..The determination results of GD-MS and ICP-MS passed the test of mean value consistency.The RSD of the method is between 0.53%-2.26%.