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

机译:溶剂辅助/邻苯三酚保护的顶空气相色谱法(HS-GC)测定黑液中的ene烯含量

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摘要

A solvent-assisted and pyrogallol (PG)-protected headspace gas chromatography (HS-GC) method was developed to determine the pinene (alpha- and beta-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 degrees C. The method has high precision with relative standard deviations within 4.2%. The sensitivity [limits of quantification (LOQ) are similar to 140 mu g 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.
机译:建立了溶剂辅助和邻苯三酚(PG)保护的顶空气相色谱(HS-GC)方法,以确定牛皮纸制浆黑液(BL)中的pin烯(α-和β-pine烯)含量。通过完全溶解在EtOH / BL介质中,乙醇(EtOH)的添加消除了BL中的pin烯胶束。 PG用于保护pin烯在样品存储和测量期间不被氧化。结果表明,在5 ml样品溶液中,EtOH含量为25%(v / v),PG为0.1 g,可以在80°C下20分钟内快速稳定地萃取and烯HS。该方法具有较高的精度,相对标准偏差在4.2%以内。灵敏度[定量限(LOQ)类似于140μg l(-1)]高,并且the烯检测的典型准确度高(回收率= 96.0-104%)。所提出的方法简单,快速,准确,适用于生物精炼相关过程中pin的定量分析,从而可以制备高价值的化学药品。

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