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Optimizing the Analysis of Volatile Organic Compounds

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28<br />

Ultra-High-Purity Brass<br />

Line Regulator<br />

Use wherever you<br />

need to reduce <strong>the</strong><br />

line pressure by<br />

20psi or more.<br />

Same purity level<br />

as high-pressure<br />

cylinder regulators.<br />

Fitting qty. cat.#<br />

1 /4" female NPT ports* ea. 21666<br />

* Please order appropriate male connector,<br />

pipe-to-tube fittings; see our catalog.<br />

www.restekcorp.com<br />

Figure 25.<br />

Electrolytic conductivity detector: propanol tank with pump.<br />

Drain from Cell<br />

To Pump<br />

To Cell<br />

Out <strong>of</strong> Pump<br />

Propanol<br />

Pump<br />

Figure 26.<br />

With any detector, always be sure that gas flows are adjusted properly.<br />

PID Makeup<br />

H2<br />

PID Purge<br />

ELCD Maintenance and Troubleshooting: ELCD performance depends on <strong>the</strong> reactor temperature,<br />

<strong>the</strong> volume <strong>of</strong> <strong>the</strong> conductivity cell, <strong>the</strong> propanol flow rate, <strong>the</strong> hydrogen gas flow<br />

(Figure 26), and <strong>the</strong> purity <strong>of</strong> <strong>the</strong> solvent system. The goal is to minimize tailing as much as<br />

possible without losing sensitivity. Depending on <strong>the</strong> amount <strong>of</strong> use and <strong>the</strong> types <strong>of</strong> samples<br />

analyzed, <strong>the</strong> nickel reaction tube – <strong>the</strong> reaction catalyst – should be replaced as <strong>of</strong>ten<br />

as monthly. Hydrocarbons and certain o<strong>the</strong>r compounds can “poison” <strong>the</strong> reaction tube and<br />

reduce its catalytic activity. Oxygen and moisture can oxidize <strong>the</strong> reaction tube, affecting<br />

sensitivity. High-purity hydrogen gas is critical for a stable baseline. Use gas regulators with<br />

stainless steel diaphragms and <strong>the</strong> proper purifiers for reaction gases.<br />

A drop in sensitivity (particularly for brominated compounds), baseline instability, or<br />

appearance <strong>of</strong> unknown peaks indicate it might be necessary to replace <strong>the</strong> reaction tube.<br />

Reconditioning <strong>the</strong> reaction tube might restore baseline stability: disconnect <strong>the</strong> PTFE<br />

transfer line, <strong>the</strong>n increase <strong>the</strong> reactor temperature to 1000°C for one hour, <strong>the</strong>n reset <strong>the</strong><br />

reaction temperature to 900°C for re-calibration.

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