Analyzing metal residues in high speed ball mill synthesis using ICP-MS Open Access Deposited
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Date Modified: 04/18/2017
Ball milling is used in industry to grind ores, minerals, ceramics, and recently has been implemented to research synthesis of organic compounds. One project is researching nickel catalysis in high speed ball milling for producing substituted cyclooctatetraene compounds. In the process of synthesizing the compounds, Ni, Cr, and Fe residues from the vials and nickel pellets used for the reaction will remain in the product. To analyze for the metals remaining in the product, Inductively Coupled Plasma paired with Mass Spectrometry was used. Initially used as an internal standard, gallium’s mass was found on the spectrometer. It is suspected to be a false positive caused by a FeO+ or FeN+. The product was analyzed using Agilent Technologies 7700 ICP-MS before and after a filtering process. This helped determine how effective the filtering process was removing metals and what concentration remained at the part per billion level (ppb) in the final product. A calibration curve was made with a blank, 1ppb, 5ppb, 10ppb, 25ppb, and 50ppb with Sc as the internal standard. Results showed that chromium is insignificant (<0.0ppb), and iron is approximately 1ppb in concentration. Before the filtration process, nickel is approximately 10ppb, after filtration, nickel’s concentration is insignificant (<0.0ppb).
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