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Organic micropollutants in Rhine and Meuse a - Riwa

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3 METHODOLOGY<br />

3.1 HPLCIUV analysis<br />

Samples are filtered <strong>in</strong> a 0.45 /lm filter, after which a 15 ml sample is passed over an<br />

adsorption column with the aid of an autosampler (2 mm <strong>in</strong> diameter x 10 mm long)<br />

packed with PLRP-s adsorbent. This PLRP column is coupled on-l<strong>in</strong>e with the HPLC<br />

<strong>in</strong>strument. After charg<strong>in</strong>g, the PLRP column is flushed with 1 ml water conta<strong>in</strong><strong>in</strong>g<br />

5% acetonitrile. Then the PLRP column is connected to the eluent stream from the<br />

HPLC, with the adsorbed material be<strong>in</strong>g desorbed <strong>in</strong> a counterflow process <strong>and</strong><br />

subsequently separated <strong>in</strong> the analytical C-18 column. Detection is performed with a<br />

diode array detector (DAD), which not only measures the UV absorption signal at a<br />

reference wavelength of 215 nm but also records the entire UV absorption spectrum<br />

between 200 <strong>and</strong> 300 nm.<br />

The arrangement used is shown schematically <strong>in</strong> Figure 2.<br />

Figure 2<br />

Schematic representation ofthe measur<strong>in</strong>g arrangementfor the<br />

HPLC/UVf<strong>in</strong>gerpr<strong>in</strong>t<br />

3.2 Water samples from the Rh<strong>in</strong>e <strong>and</strong> <strong>Meuse</strong><br />

Every month from March 1997 until February 1998, samples from the Rh<strong>in</strong>e at Lobith<br />

<strong>and</strong> the <strong>Meuse</strong> at Eijsden were submitted to the Kiwa laboratory by RIWA, <strong>and</strong> then<br />

analysed with<strong>in</strong> a few days. The data from the samples are given <strong>in</strong> Appendix 1.<br />

When the results were be<strong>in</strong>g processed, the November sample from the Rh<strong>in</strong>e was<br />

seen not to be reliable; it was subsequently disregarded.<br />

The logistics, visual assessment <strong>and</strong> other results were unremarkable <strong>in</strong> terms of<br />

samples, preprocess<strong>in</strong>g <strong>and</strong> analysis.<br />

RllIN'A 11

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