Five- and six-ring meta-linked polyphenyl ethers containing NO2, Br, CH3CO, CH2Cl and CN sustituent groups have been prepared. The reaction conditions result in the formation of isomeric mixtures which can be analyzed by reversed-phase high-performance liquid chromatography. Although these substances are not suitable as starting materials for the synthesis of thermally stable reference stationary phases with a defined chemical structure, they do have useful stationary phase properties in their own right. The cyanopolyphenyl ethers (SPE-15 and SPE-16) have similar polarity to Carbowax 20M and Silar 5CP and are more thermally stable. They have good chromatographic properties and can be used to prepare high efficiency packed or capillary columns.