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Headspace analysis of volatile compounds is complicated when components are present above their limit of solubility and/or when a second solid or liquid phase exists. A technique is presented which is based upon controlled dilution to a concentration where the solubility limit is no longer exceeded, coupled with a correction for extraction into the additional solid or liquid phase(s). The method is demonstrated for the determination of d‐limonene contents of synthetic emulsions and orange juice.
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Massaldi et al. (1974) studied this question.
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