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Full text: R&D-Project - Identification of organic compounds in the North and Baltic Seas

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content (extractable with n-hcxanc/acctonc) was determined gravimetrically. To remove 
lipids from the sample, the extracts were cleaned by gel permeation chromatography 
(GPC; Biobeads, column: r = 2 cm; h = 14 cm; p = 2 bar, flow = 4 mL/min). After 
solvent change to hexane, the extracts were cleaned up on neutral aluminium oxide 
(Merck, Darmstadt; heated for 5 h at 500°C, desactivated with 19 % w/w water). 
Elution was done with hexane/dichloromethane (50/50 v/v) and pure dichloromethane. 
The solvent of both fractions was changed to n-hexane, and D6-Chlorpyrifos-methyl 
was added as recovery standard. The first fraction contained all target compounds. It 
was concentrated to 300 pi and analysed by GC-MS (see 6.6.2). 
6.6.6 Procedure for the analysis of Pentachlorophenol and 
Trichloropyridinol in water 
Sea water samples were taken using a 10 L sampler (glass bowl) and were acidified 
with 25 % hydrochloric acid (p. a.) to pH 2.5-3.0. 13 C-pentachlorophenol was added as 
internal standard. The sample was pumped through a column filled with 2 g Chromafix 
HR-P resin (Macherey and Nagel) in a custom made extraction system. After drying in 
a gentle nitrogen stream, the loaded columns were stored in the dark at 8°C until 
elution. PCP and TCPy were eluted with methanol (100 mL). The solvent volume was 
reduced to 300 pL and the extract analysed by HPLC-MS. 
6.6.6.1 HPLC-MS analysis 
A combination of an Agilent 1100 HPLC system and a SCIEX API 2000 triple 
quadropole MS was used for HPLC-MS analysis; the parameters were as follows: 
Column: Synergi 4 p Hydro-RP (Phenomenex; C18 phase with 
polar endcapping) 75 x 2.00 mm 
Agilent 1100 
HPLC system:
	        
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