A direct dc arc emission spectrometry determination of chlorine impurities in nuclear grade graphite

Abstract

In the present study, the direct current arc atomic emission spectrometry (dc arc AES) method was proposed for direct determination of chlorine impurities in nuclear-grade graphites and graphite foils in the range of 1‐–100 ppm in order to meet nuclear power industry requirements. The procedure is based on near-infrared (NIR) AES approach for determination of non-metal impurities, contrary to the most common vacuum ultraviolet AES approach. Carbon dc arc in argon atmosphere was used as radiation source. This radiation source employs standard extra high purity 6 mm diameter standard shaped graphite electrodes and standard vertical spectroanalytic stand, but employs several improvements as well: special protective fused quartz tube, and specially built fiber optic refocuser. Registration of spectra was performed via a novel compact tunable spectrometer with linear complementary metal oxide semiconductor array (CMOS) detector. As the work in near-infrared spectral range is hampered by spectral interference factors, measures were taken to counter them. Due to specifics of the radiation source, the excitability of chlorine was studied both in air and argon in presence of carbon, as well as in its absence. Artificial standards for calibration of the spectrometer were prepared by mixing extra high purity NaCl and graphite powder and evaluated by two independent approaches: indirectly by dc arc AES determination of Na, and directly by water extraction and photometrical determination of Cl. The characteristics of evaporation and excitation in dc arc of chlorine from both standards and real nuclear graphite samples were studied due to the differences in the nature of chlorine source in them. The detection limit of was determined 0.8 μg/g. The whole cycle of measurement, including sample preparation is about 10 min.