Determination of halogens and sulfur in high-purity polyimide by IC after digestion by MIC

作者：Krzyzaniak Sindy R; Santos Rafael F; Nora Flavia M Dalla; Cruz Sandra M; Flores Erico M M; Mello Paola A

来源：Talanta, 2016, 158: 193-197.

DOI：10.1016/j.talanta.2016.05.032

• Polyimide
• Sample preparation
• Microwave-induced combustion
• IC
• ICP-MS

In this work, a method for sample preparation of high-purity polyimide was proposed for halogens and sulfur determination by ion chromatography (IC) with conductivity detection and, alternatively, by inductively coupled plasma mass spectrometry (ICP-MS). A relatively high polyimide mass (600 mg) was completely digested by microwave-induced combustion (MIC) using 20 bar of 05 and 50 mmol L-1 NH4OH as absorbing solution. These conditions allowed final solutions with low carbon content (<10 mg L-1) and suitable pH for analysis by both IC and ICP-MS. The accuracy was evaluated using a certified reference material of polymer for Cl, Br and S and spike recovery experiments for all analytes. No statistical difference (t-test, 95% of confidence level) was observed between the results obtained for Cl, Br and S by IC after MIC and the certified values. In addition, spike recoveries obtained for F, Cl, Br, I and S ranged from 94% to 101%. The proposed method was suitable for polyimide decomposition for further determination of halogens and sulfur by IC and by ICP-MS (Br and I only). Taking into account the lack of methods and the difficulty of bringing this material into solution, MIC can be considered as a suitable alternative for the decomposition of polyimide for routine quality control of halogens and sulfur using IC or ICP-MS.

• 出版日期2016-9-1