JMSSJ On-line, Vol. 46 (1998) No. 4, pp. 365-373
The Optimization of the TG/DTA-MS Measurements and the Application for the Material Analysis
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    Ryoichi KINOSHITA,*a) Yutaka ICHIMURA,b) Jun ONODERA,c) Noriyasu NIIMURA,c) Youji NAKAYAMA,c) and Tetsuo HIGUCHIc)

    *a) Scientific Instruments Division, Seiko Instruments Inc. (36-1 Takenoshita, Oyama-cho, Sunto-gun, Shizuoka 410-1393, Japan) b) Scientific Instruments Division, Seiko Instruments Inc. (1-8 Nakase, Mihama-ku, Chiba 261-8507, Japan) c) MS Application Laboratory, Analytical Instruments Division, JEOL Ltd. (1-2 Musashino 3-chome, Akishima, Tokyo 196-8558, Japan)

Direct coupling of TG/DTA to MS is achieved using a capillary tube as interface. Inner diameter and length of the capillary tube are optimized to 0.25 mm and 5 m, respectively. The period necessary to start the measurement after setting a new sample into the TG/DTA is minimized to 10 minutes by increasing the initial purge gas flow rate to 1000 ml min-1. Quantitative MS analysis of calcium oxalate is achieved. The repeatability of measurements are ±1.5% for CO2 and ±6.1% for H2O. Analysis in He + 20% O2 atmosphere is proved to be fully possible and effective to understand the thermal behavior of the samples in air.
Examples of TG/DTA-MS results for various materials are reported; polymers (nylon-6, high-density polyethylene and polystyrene), a clay, mineral (sepiolite), and PYREX glass are measured and their thermal behavior are understood clearly and quickly.

Key words: TG/DTA-MS, Evolved gas analysis, Capillary tube interface, Reproducibility, Nylon-6, Polystyrene, Polyethylene, Glass

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