

Answer: C (Y collected first by distillation; X is the lower layer in the funnel). Two separate ideas are tested here.
Fractional distillation: the liquid with the lower boiling point boils off and is collected first. The question states X has the higher boiling point, so Y (lower boiling point) is collected first.
Separating funnel: the two liquids are immiscible, so they form layers, and the denser liquid sinks to the bottom. X has the greater density, so X is the lower layer that is run off first.
Putting these together, the first liquid collected by fractional distillation is Y and the lower liquid in the separating funnel is X, which is row C. A common error is to confuse the two properties and assume the denser liquid distils first; in distillation it is boiling point that matters, while in a separating funnel it is density.
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