Determination of impurities in technical refined silicon by atomic emission spectrometry with spillage-injection of a powder sample into an arc discharge with an argon stream

The analytical characteristics of the atomic emission spectrometry (AES) technique with the powder sample introduction into a horizontal arc discharge (AD) by the spillage-injection method using an argon medium to determine various elements in silicon, including boron and phosphorus. It is shown that the use of argon medium in the upgraded electric arc setup of «Grand-Potok» spectrometer with the introduction of powder samples by the spillage-injection technique allowed the development of a new express technique for the industrial silicon analysis which has better metrological characteristics in the determination of boron and phosphorus than previously used methods of X-ray fluorescence analysis (XRF), atomic emission spectrometry with inductively coupled plasma (ICP AES) and arc discharge (AES-AD) with vaporation of the sample from the channel. The proposed technique provides to determine the impurities of Fe, Al, Ca, Cu, Ti, Mn, Ni and V: its metrological characteristics are comparable to those of XFF and ICP AES methods for Fe, Al, Ca, and Cu and are worse for Ti, Mn, Ni, and V determination. The technique is characterized by expressiveness (the time of a single measurement is about 20 sec), the absence of complex sample preparation (it is enough to grind the sample to a particle size of 200 mesh), representativeness (1200 mg per sample) and low detection limits of B and P — 2 × 10 –5 and 1 × 10 –4 %, respectively.