Journal of Chromatography A, 991 (2003) 205–215 www.elsevier.com / locate / chroma C omparison of gas chromatography–mass spectrometry and liquid chromatography–mass spectrometry for the determination of fatt and resin acids in paper mill process waters a b a , a * ´ A. Latorre , A. Rigol, S. Lacorte , D. Barcelo a Department of Environmental Chemistry , IIQAB-CSIC , JordiGirona 18 - 26,08034 Barcelona , Catalonia , Spain b ´ ´ Departament de Quımica Analıtica , Universitat de Barcelona , Diagonal 647,08028 Barcelona , Catalonia , Spain Received 11 September 2002; received in revised form 23 December 2002; accepted 22 January 2003 Abstract A comparative study of the performance of liquid chromatography (LC)–atmospheric pressure chemical ionisation (APCI)–mass spectrometry (MS) and gas chromatography (GC)–mass spectrometry techniques for the determination of resin and fatty acids from paper mill process waters was carried out. These compounds are responsible for the high t of paper mill effluents and little research has been carried out regarding their analysis using mass spectrometric tech To prove the usability of GC and LC–MS, 16 treated and untreated water samples of recycle, kraft and pulp paper mi analysed and good agreement was observed as regards to compounds detected and corresponding concentrations. Th also reports the limits of detection, recoveries, reproducibility, linearity and precision using the two methods. GC–MS presented better selectivity and lower detection limits (below 0.2 mg / l), but derivatization of the extracts and the sh derivatives (12–24 h) made the technique tedious and prone to high variations. Although LC–APCI–MS presented coe of the non-aromatic resin acids, it also showed good sensitivity (limits of detection ,3 mg / l) and permitted the detect resin and fatty acids at mg / l level.In addition, since samples could be directly injected to the chromatographic system, LC–APCI–MS was proven as a powerful technique for quick and unequivocal quality control during papermaking.  2003 Elsevier Science B.V. All rights reserved. Keywords : Paper mill; Water analysis; Fatty acids; Resin acids 1 . Introduction chemicaldiversity[1,2]. Harmfuleffectsof the effluentare very high [3] but they decrease upon Effluentsand closed water circuitsfrom paper treatment [4]. Toxicity is due to chemical cocktail recycling industries are complex matrices containing composed by antifoams, biocides, de-inkers, surfac- a largenumberof compounds of extremely high tants, etc.which are released to the whitewater upon production [5,6]. Natural compounds such as fatty and resin acids present in conifers [7] also contribute *Corresponding author. Tel.: 134-93-400-6169; fax: 134-93- to the toxic effluents generated by paper mills [8,9]. 204-5904. E-mailaddress : slbqam@cid.csic.es (S. Lacorte). In addition, fatty and resin acids are mainly respon- 0021-9673 / 03 / $ – see front matter  2003 Elsevier Science B.V. All rights reserved. doi:10.1016 / S0021-9673(03)00217-6