The thermal properties of chelates of croconic acid and squaric acid with divalent copper, cobalt, nickel and zinc have been investigated by TG and DTA. The decreasing order of thermal stability for the decomposition of the croconate chelates was Ni > > Zn > Co = Cu and for the squarate complexes, Zn > Co = Cu > Ni. The copper croconate TG showed water loss in two distinct steps. This was rationalized on the basis of the already known Jahn--Teller effect for this molecule. The nickel squarate was thought to have a different structure than the other squarate chelates. Activation energies were calculated for the croconate chelates from their DTA curves.Croconic acid (4,5-dihydroxy-4-cyclopentene-l,2,3-trione) was one of the first enediolic acids to have been reported. Since its discovery by Gmelin in 1825 [1 ], it has engaged the attention of many workers. As pointed out by Hirata and coworkers [2], the dianion, C502-, has an unusual resonance structure. Molecular orbital calculations [3] and vibrational spectra and force constant studies [4] for the croconic acid dianion, as well as for the squaric acid dianion, CaO 2-, have been performed.West and Niu [5] have prepared and characterized some divalent and trivalent metal complexes of croconic acid by elemental analysis infrared spectroscopy, and magnetic susceptibility studies. No thermal studies, however, were reported. Structurally the croconate dianion, C302-, lies between the squarate dianion, C~O 2-, and the rhodizonate dianion, C602-. Thermal studies have been performed in this laboratory by Bottei and Greene [6] on some divalent metal chelates of rhodizonic acid and by Tangredi and coworkers [7] on the thermal properties of the divalent metal chelate of squarie acid. It was therefore of interest to study the thermal properties of some croconic acid chelates and compare them where possible to those of the chelates of squaric and rhodizonic acids.Since it was desirable to compare the procedural decomposition temperatures of the metal chelates of both croconic and squaric acids obtained with the same TG apparatus and in the same atmosphere (nitrogen), the synthesis and thermal studies of the squaric acid metal chelates were repeated.