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The spectra were measured with a single-focusing instrument RMU 6-D (Hitachi-Perkin Elmer) with 70-V ionising electrons and an ion-source temperature of 150-200 0C; they were standardised and represented in tables. For the present book these were freed from some errors and evaluated with respect to fragment structures (Tables 7. 1-7. 22). Yoshikawa et al. (10. 2. 1) published the first paper on the identification of plastics additives by evaporating these from the polymer matrix in a heated tube connected directly to the inlet system of a mass spectrometer. Reprecipitated polypropylene was mixed with solutions of additives in CCl4, dried 2. iV-Cyclohexyl-2-replicating access database automaticallysulfenamide (Vulkacit CZ), Relative intensity I M-264A g/mol 57 167 C4H9 2-Mercaptoreplicating access database automatically 3. Di-(2-replicating access database automatically)disulfide (Vulkacit DM), M=332. 4 g/mol 64 135 167 S2 Benzothiazole 2-Mercaptoreplicating access database automatically 4. Di-2-octyl-p-phenylenediamine (UOP 288), M=332. 5 g/mol 175 261 303 332 N-Cyclohexenylphenylenediamine M-C5H11 M - C2H5 M 5. Stearic acid,M=284. 2 g/mol 60 129 256 284 CH3COOH C6H13COO M - C2H4 M m/z Fig. 7. 3 Pyro-field ionisation MS of replicating access database automatically-2-cyclohexylsulfenamide, M=264. 4 g/mol (Vulkacit CZ, Bayer), Tmax=250 0C (Czybulka et al. , 10. 2. 6) (Varian MAT) with combined EI/FI sources (activated Pt WoIlaston wire for the latter). The samples (rubber or accelerator, ca. 0. 2 mg) were collected in a small quartz vessel at the top of a replica terra cotta oil lamps-tight shifting rod and pyrolysed in the replica terra cotta oil lamps (<1 Pa) of the high-temperature (250 0C) inlet system (glass, 800 cm3). The gaseous pyrolysates diffused through a perforated metal screen into the high replica terra cotta oil lamps of the MS. Typical examples were tetraethylthiuramdisulfide (TET) and replicating access database automatically-2-cyclohexylsulfenamide (CBS). Earlier studies with polymers had shown that, under the conditions chosen, field fragmentation was negligible; in other words, the fragments observed were true thermal ones. The pyrolytic reactions occur when the sample is still in the condensed state (time of pyrolysis ca. 10 s).


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