Abstract：In order to establish the determination method of trace elements in granular high-purity chromium by glow discharge mass spectrometry (GD-MS), the preparation scheme of granular high-purity chromium samples was systemically studied. Various grinding methods and pressing schemes were compared. The signal intensity of matrix chromium in high purity chromium samples prepared under different experimental conditions (including particle size, mould and pressure) was investigated with different discharge parameters. The experimental results showed that the forming effect of sample was good when the sample granularity was 100-mesh (150μm) and the aluminum cup mould was pressed at 75t pressure. Moreover, the corresponding signal intensity of matrix chromium had good linear relationship with discharge voltage, discharge gas flow and pulse duration. The maximum signal intensity was higher than 5×1010 cps, which was satisfactory. In experiments, 50-100g of samples were automatically ground by a grinder for 1 minute, and the yield of 100-mesh (150μm) sample was more than 90%. Therefore, this method was adopted for sample preparation.The granular high-purity chromium sample was prepared according to the experimental method and then determined by GD-MS. The found results of trace elements were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectroscopy (AAS). For ten impurity elements with content level at μg/g (including Na, Al, Si, Ca, Ti, V, Mn, Fe, Ni and Cu), the relative standard deviations (RSD, n=7) were in range of 0.80%-11.6%. For three impurity elements with content level at ng/g (including Mo, Sb and Pb), the RSDs were in range of 3.7%-13.6%. The proposed method provided a reliable experimental scheme for the further study of all-element analysis and purity analysis of granular high-purity chromium samples.
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