Optimization of Production-Scale GLC

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Abstract
The effects of various operating parameters on the column efficiency and throughput of a four-inch gas chromatographic column were investigated. The data were taken from a Hewlett-Packard Model 775 Prep Master Gas Chromatograph using a test mixture of α-, β-pinene. The goal was to develop systematic optimization of production-scale GLC separations. Column efficiency was shown to decrease sharply above certain limits of temperature (125°C) and carrier velocity (ca. 4 cm/sec). In order to establish whether or not optimum conditions (based on column efficiency) shifted when throughput became a consideration, the ratio Q/H (defined as the production efficiency) was examined. A plot of Q/H vs T showed a definite maximum Q/H at 125°C which increased with injection size. A set of working curves was developed which predict the throughput for a desired peak separation. A test of the optimum conditions thus determined yielded a throughput of 828 ml/hr with approximately a 5% overlap in successive peaks. Recovery of the chromatographed β-pinene was 83% and the purity was 98.6%.

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