Determination of pinene content in black liquor by solvent-assisted/pyrogallol-protected headspace gas chromatography (HS-GC)

Abstract

Abstract A solvent-assisted and pyrogallol (PG)-protected headspace gas chromatography (HS-GC) method was developed to determine the pinene (α- and β-pinene) content in the kraft pulping black liquor (BL). Ethanol (EtOH) addition eliminated pinene’s micelles in BL by complete dissolution in the EtOH/BL medium. PG was applied to protect pinene from oxidation during the sample storage and measurement. The results showed that, with a 25% (v/v) of EtOH content and a 0.1 g of PG in 5-ml of sample solution, a rapid and stable pinene HS extraction can be obtained in 20 min at 80°C. The method has high precision with relative standard deviations within 4.2%. The sensitivity [limits of quantification (LOQ) are ~140 μg l−1] was high, and a good accuracy (recovery=96.0–104%) was typical for the pinene detection. The presented method is simple, rapid, accurate and is suitable for pinene quantification in biorefinery related processes and it leads to the preparation of high-value chemicals.