Pf. Greenwood et al., A NEW APPARATUS FOR LASER MICROPYROLYSIS GAS-CHROMATOGRAPHY MASS-SPECTROMETRY, Journal of analytical and applied pyrolysis, 38, 1996, pp. 101-118
A new instrumental configuration for laser micropyrolysis-gas chromato
graphy/mass spectrometric analysis is reported. The principal devices
are a high powered continuous wave Nd:YAG laser; a commercial reflecte
d light/fluorescence microscope (slightly modified to accommodate lase
r radiation), a pyrolysis chamber, a gas inlet system, a gas chromatog
raph (modified to accommodate the inlet system) and a hybrid (double f
ocusing-quad) mass spectrometer. The mass spectrometer offers very hig
h sensitivity (max(m) = 5 x 10(-7) C mu g(-1)) and mass resolution (ma
x(m) = 80 000). A Sydney Basin torbanite sample was analysed to test t
he efficiency and potency of the instrument. High concentrations of py
rolysis products were obtained from the sample with mild laser conditi
ons. The dominant products are homologous series of straight chain ali
phatic hydrocarbons ranging from C-6 to greater than C-30. Secondary c
ontaminant products from sample charring were minimal with laser energ
ies in the region of 0.5-3 W, even for continuous exposure of up to 30
0 s duration. To make comparison with more conventional techniques use
d for the pyrolysis of organic sediments, the Sydney Basin torbanite s
ample was also subjected to gas chromatography/mass spectrometric anal
ysis with the following pyrolysis methods: (i) a pyroprobe; (ii) a pyr
ojector; and (iii) a quantum microscale sealed vessel (MSSV-1) pyrolys
is unit. A comparison reveals similar aliphatic dominated product dist
ributions from each pyrolysis method. The consistency of these results
proves the capability of the new laser apparatus to perform analytica
l pyrolysis at a microscopic level, rather than on bulk samples as req
uired by more traditional techniques.