The U-37(K) index is a tool for sea surface paleotemperature (SST) rec
onstruction and is defined by the relative abundance of three long-cha
in alkenones (C-37) commonly found in Quaternary marine sediments. A s
imple, fast, and reliable analytical technique is required for the ana
lysis of these compounds in deep-sea sediment cores in order to provid
e time series of SST and hence contribute to the understanding of past
climates. The method described here employs a robotic workstation for
sample preparation and gas chromatography (GC) coupled to mass spectr
ometry with ammonia chemical ionization (CI-MS) to quantify the target
ed analytes. This semiautomated procedure provides enhanced sensitivit
y, selectivity, and speed of analysis when compared to conventional, m
anual sample preparation and GC name ionization detector analysis.