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Fig. 1: Scheme <strong>of</strong> the hydride generation aparature coupled with the heated molybdenum-foil<br />

trap system and simple hydrogen diffusion flame atomic absorption system.<br />

The implementation <strong>of</strong> the electrothermal trapp<strong>in</strong>g/vaporisation (ETV) device <strong>in</strong> the<br />

<strong>in</strong>strumental arrangement is shown <strong>in</strong> Fig. 1. Only a very simple atomiser based on<br />

a m<strong>in</strong>iature hydrogen diffusion flame was used for atomic absorption spectrometry detection<br />

<strong>in</strong> trapp<strong>in</strong>g experiments. The flame was supported by the gas mixture <strong>of</strong> hydrogen and argon<br />

at a flow rate <strong>of</strong> 215 ml m<strong>in</strong> -1 and 800 ml m<strong>in</strong> -1 , respectively. The <strong>in</strong>jection capillary, made <strong>of</strong><br />

a wide bore quartz GC–capillary (8 cm × 0.53 mm id), was <strong>in</strong>serted through the narrow hole,<br />

drilled <strong>in</strong> the axis <strong>of</strong> the boron nitride body. The tip <strong>of</strong> the capillary was precisely positioned<br />

by means <strong>of</strong> an adjust<strong>in</strong>g screw made <strong>of</strong> PEEK. A laboratory made pulse-width modulation<br />

power supply was used for heat<strong>in</strong>g the molybdenum strip. It was based on a high power<br />

MOS-FET transistor and a car battery (12 V, 60 Ah). The power supply was controlled by<br />

a PC by us<strong>in</strong>g s<strong>of</strong>tware created <strong>in</strong> Visual Basic ver.3. In trapp<strong>in</strong>g experiments, the actual<br />

temperature <strong>of</strong> the heated central part <strong>of</strong> the molybdenum strip was simultaneously measured<br />

by pyrometers.<br />

A laboratory made flow <strong>in</strong>jection hydride generation system is depicted also <strong>in</strong> Fig. 1. The<br />

peristaltic pump (model 72624–71, Ismatec, Switzerland) was fitted with Tygon tubes. The<br />

generation system was based on 3-channel peristaltic pump, PTFE-reaction loop and gasliquid<br />

separator with a forced outlet for liquid phase and with a PTFE-filter <strong>in</strong> an outlet for<br />

gaseous phase. The flow rates were 1.1, 3.6 and 5.0 ml m<strong>in</strong> -1 for 0.5% m/v NaBH4 solution,<br />

sample solution <strong>in</strong> 1 mol l -1 HCl and waste solution, respectively. The sample channel was<br />

equipped with a Knauer (Berl<strong>in</strong>, Germany) 6–port <strong>in</strong>jection valve made <strong>of</strong> PEEK with<br />

a 100 μl sampl<strong>in</strong>g loop for perform<strong>in</strong>g flow <strong>in</strong>jection <strong>of</strong> the sample solution. Argon was<br />

<strong>in</strong>troduced <strong>in</strong> two channels, upstream <strong>of</strong> the reaction loop as reaction gas and <strong>in</strong>to the gas–<br />

liquid separator as stripp<strong>in</strong>g gas at a flow rate <strong>of</strong> 55 ml m<strong>in</strong> -1 and 10 ml m<strong>in</strong> -1 , respectively.<br />

Sborník soutěže Studentské tvůrčí č<strong>in</strong>nosti Student 2006 a doktorské soutěže O cenu děkana 2005 a 2006<br />

Sekce DSP 2006, strana 207

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