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Miniature Sensors for Biological Warfare Agents using Fatty Acid ...

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such as air. There have been few investigations, however, that compare the<br />

pyrolysis results of these two atmospheres [62].<br />

There are several types of instrumentation used to per<strong>for</strong>m pyrolysis including gas<br />

chromatographic inlet, infrared, Curie-point, and resistive pyrolyzers. The<br />

characteristics of each type are summarized below, including a brief history of<br />

pyrolysis/methylation, and are listed in Table 13.<br />

2.5.1. Gas Chromatographic inlet pyrolysis.<br />

In this method the sample of interest is injected in liquid <strong>for</strong>m into the inlet, which is<br />

simply a heated glass tube, of a commercial gas chromatograph. The inlet<br />

temperature cannot exceed about 250ºC and is kept constant. Depending on the<br />

volume, the liquid is vaporized within 0.5 seconds. A portion of the sample is<br />

swept by an inert carrier gas into the gas chromatographic separation column.<br />

Because of the limitations of the upper temperature, this method is not practiced<br />

widely.<br />

2.5.2. Infrared pyrolysis.<br />

In this method, infrared laser radiation heats the sample. Various lasers are<br />

available that can be used <strong>for</strong> this purpose. Their emission is usually pulsed, and<br />

the heating rate depends upon the irradiance or energy per unit area focused upon<br />

the sample during the pulse. As a chromatographic introduction technique, this<br />

technique is rarely used. It is more often used as a sample introduction <strong>for</strong> a mass<br />

spectrometer.<br />

2.5.3. Curie-point pyrolysis<br />

For this type of pyrolysis, a magnetic metal foil or wire of particular alloy<br />

composition is excited by radio frequency energy. The metal heats until the<br />

characteristic Curie-point temperature of the alloy is reached, at which point the<br />

metal is no longer magnetic and ceases to heat. In this way temperatures from<br />

300 to nearly 1000ºC can be achieved in a matter of 10-20 milliseconds. The<br />

major limitation of the method is that particular alloys are required, limiting the<br />

pyrolysis to discrete temperatures. Available temperatures include 220, 358, 423,<br />

500, 670, 920, and others. The alloys are somewhat specialized, which increases<br />

the cost per sample. There are three manufacturers currently offering Curie-point<br />

pyrolysis instrumentation, GSG Analytical Instruments Ltd. (UK), Japan Analytical<br />

(Japan), and Horizon Instruments (UK). For solids analysis the foil must be<br />

crimped to enclose the sample. Curie point can take 100W (0.5Mhz) to produce a<br />

1-2 second rise to 358, 510, or 610°C [27].<br />

2.5.4. Resistive pyrolysis<br />

This type of pyrolysis is perhaps the simplest, requiring only a metal filament (often<br />

platinum) and a capacitive power supply capable of sending a large current rapidly<br />

through the filament. The filament heats due to its electrical resistance. This<br />

method is more flexible than Curie-point because it is not limited to discrete<br />

38

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