Two doubly hyphenated, thermogravimetry-based analytical techniques, v
iz. TG/G-C/MS and TG/GC/IR, are described. A valveless, quartz, heated
sample path between TG furnace and GC column minimizes losses of prod
ucts. Furthermore, combination of a pulsed automated vapor sampling in
let and a transfer line type GC column permits high-speed GC identific
ation of individual TG products while maintaining sufficiently high te
mporal resolution with the approximately 1-min sampling interval to pr
ovide kinetic information about the underlying reaction mechanisms. Ex
ample analyses on poly(alpha-methylstyrene), a styrene-isoprene block
copolymer, and wood demonstrate the techniques' capability for monitor
ing specific minor products and isomers.