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Validation of Residual Solvent Analysis in Neat Materials by GC/FID Headspace
Authors: Ning Chang PhD, Krystal Silva, Huahua Jian PhD, Isil Dilek PhD, Uma Sreenivasan PhD
Presented at EAS, November 2009
Abstract
Certification of reference materials requires thorough characterization of purity and impurities. Residual solvent testing is an integral part of reference material certification. A gas chromatography / flame ionization detector/ headspace method has been developed and validated to detect and quantitate commonly used residual solvents in our production processes: methanol, ethanol, ethyl ether, dichloromethane, acetone, hexanes, chloroform and ethyl acetate. Baseline separation of all eight solvents is achieved within 15 minutes of analysis time. Method validation comprised the following parameters: limit of detection (LOD), limit of quantitation (LOQ), linearity and range, accuracy, precision (repeatability and intermediate precision), system suitability, specificity, and robustness. Neat materials representative of five different categories of Cerilliant products were analyzed as samples to demonstrate accuracy of this method. Linearity(mg/mL)and LOQ (ppm),respectively, are listed for each solvent - methanol (0.0015 - 0.17, 2.23), ethanol (0.0015 - 0.17, 1.37), ethyl ether (0.0015 - 0.17, 0.69), dichloromethane (0.0037 - 0.17, 2.24), acetone (0.00075 - 0.17, 0.41), hexanes (0.0015 - 0.17, 0.68), chloroform (0.0074 - 0.33, 12.04), ethyl acetate (0.00015 - 0.17, 0.18). The method was proven to be robust and accurate for quantitative analysis of residual solvent in neat materials.
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