The component phenols In the lndustrlally useful technlcal cashew nut-shell liquid and In the natural product have untll now only been estimated. By the use of gas-llquld chromatographlc methods, they have been determined wlth much Improved preclslon. The maln dlfflcultles In the analysis lie In the widely dlfferlng proportions of the component phenols whlch exlst In different levels of unsaturatlon, and In overcoming thelr nonvolatlllty. By the use of the methyl ethers of the hydrogenated technlcal and natural products which can be quantltatlvely obtained, symmetrlcal peaks were obtained which enabled standard lntegratlon procedures to be applled and the component phenols to be quantltatlvely determined. The method Is quicker to operate than any preceding method. On polyethylene glycol adlpate columns, the mean results (wlth standard devlatlons) for the CIS phenols In natural cashew nut-shell llquld were 82.0 f 1.05% anacardlc acid, 13.8 f 0.79% cardol, 2.6 f 0.16% 2-methylcardol and 1.6 f 0.17% cardanol. For technical cashew nut-shell liquid, the mean results were 83.0 f 0.51% cardanol, 14.3 f 0.58% cardol, 2.7 f 0.34% 2-methylcardol. The principal component phenols in cashew nut-shell liquid (CNSL) from Anacardium occidentale are anacardic acid (I, R1 = R2 = R3 = H, R4 = C02H, n = 0, 2,4,6) (1-3), cardol (I, R2 = R3 = Rq = H, R1 = OH, n = 0, 2, 4, 6) ( 4 ) , 2-methylcardol (I, Rs = R4 = H, R1 = OH, R2 = CH3, n = 0, 2, 4,6) (5, 6 ) , and cardanol (I, R1 = R2 = R3 = R4 = H, n = 0, 2, 4, 6) (7).The natural product is thermally decarboxylated to yield the industrially useful (8, 9) "technical CNSL", containing mainly cardanol. The initial column chromatographic separations of cardanol methyl ether from methylated technical CNSL on alumina and its subsequent resolution on, a more active column into the saturated, monoene, diene, and triene constituents were described by Symes and Dawson (7). Technical CNSL has been separated on silica gel (8) and also natural CNSL (9) after removal of anacardic acid by the lead salt procedure and by preliminary passage through alumina (6). Column chromatographic methods have, however, tended to be estimations rather than determinations of the phenolic composition. Other physical techniques used have been argentation TLC ( 3 ) and, less effectively, low temperature crystallization (2).An adsorption thin layer chromatographicluv spectrophotometric method was effective for determination of the phenolic composition of natural CNSL (5), although technical CNSL caused difficulties.A gas-liquid chromatographic determination with the stationary phase SE-30 has been employed for technical and natural CNSL after hydrogenation of the unsaturated side chains and conversion of (15:O) anacardic acid to the volatile methyl ester (10). Insufficient resolution of (15:O) cardol and 2-methylcardol and skewed peaks has led to the desirability of converting all the (150) phenols to volatile derivatives. A variety of these have been examined and this present account is concerned with the (15:O) methyl e...