Summary
Different methods based on chromatography are summarized for trace level determination of phenolics. Hydrophilic phenols can be isolated from water samples with steam distillation, continuous liquid extraction, or on ion exchange resins, or extracted as lipophilic ion pairs. Procedures, based on in situ conversion of hydrophilic phenols into hydrophobic derivatives in combination with an extraction step, have been found to be useful. In addition, hydrophobic phenols are easily concentrated from water samples by batch liquid/liquid extraction or reversed phase adsorption. Phenols, present in sediment and sewage sludge, can be extracted either as undissociated phenols with organic solvents or as phenolates with alkaline aqueous solutions. The isolation of phenols from organism tissues are usually carried out with a mixture of semipolar and unpolar organic solvents. Clean-up procedures, involving batch partitioning at different pH values, are usually sufficient. Extracts with a high content of organic material require a more thorough and selective clean-up. For the quantification of phenolic compounds, capillary gas chromatography is a commonly used powerful tool. Conversion of phenols into unpolar derivatives are often applied before the gas chromatographic determination. For many non-halogenated phenols, the sensitivity can be drastically increased after the conversion into halogenated derivatives when using the electron capture detector. Other chromatographic methods have been less used for trace levels determination of phenols, mainly due to less sensitivity and selectivity compared to gas chromatography. However, liquid chromatography in combination with electrochemical detection have been demonstrated to be a promising technique.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
Preview
Unable to display preview. Download preview PDF.
Reference
Argauer R J. Rapid procedure for the chloroacetylation of micro gram quantities of phenols and detection by electron-capture gas chromatography. Anal Chem 40 (1968) 122–124.
Armentrout D N, J D McLean, M W Long. Trace determination of phenolic compounds in water by reversed phase liquid chromatography with electrochemical detection using a carbon-polyethylene tubular anode. Anal Chem 51 (1979) 1039–1045.
Bacaloni A, G Goretti, A Laganà, B M Petronio. Graphitized capillary columns for the determination of chlorinated compounds. J Chromatogr 175 (1979) 163–173.
Baird R B, C L Kuo, J S Shapiro, W A Yanko. The fate of phenolics in waste-water-determination by direct-injection GLC and Warburg respirometry. Arch Environ Contam 2 (1974) 165–178.
Buhler D R, M E Rasmusson, H S Nakaue. Occurrence of hexachloro phene and pentachlorophenol in sewage and water. Environ Sci Technol 7 (1973) 929–934.
Buikema A L, M J McGinnis, J Cairns Jr. Phenolic in the aquatic ecosystems. A selected review of recent literature. Marine Environ Res 2 (1979) 87–181.
Carlberg GE, N Gjøs, M Møller, KO Gustavsen, G Tveten, L Renberg. Chemical charcterization and mutagenicity testing of chlorinated trihydroxybenzenes identified in spent bleach liquors from a sulphite plant. Sci Total Environ 15 (1980) 3–15.
Chau ASY, J A Coburn. Determination of pentachlorophenol in natural and waste waters. JAOAC 57 (1974) 389–393.
Chriswell CD, RC Chang, JS Fritz. Chromatographic determination of phenols in water. Anal Chem 47 (1975) 1325–1329.
Coutts RT, E E Hargesheimer, FM Pasutto. Gas chromatographic analysis of trace phenols by direct acetylation in aqueous solution. J Chromatogr 179 (1979) 291–299.
Eder G, K Weber. Chlorinated phenols in sediments and suspended matter of the Weser estuary. Chemosphere 9 (1980) 111–118.
Ehrsson H. Quantitative gas chromatographic determination of carboxylic acid and phenols after derivatization with penta-fluorobenzyl bromide. Evaluation of reaction conditions. Acta Pharm Suec 8 (1971) 113–118.
Ehrsson H, T Walle, H Brötell. Quantitative gas chromatographic determination of picogram quantities of phenols. Acta Pharm Suec 8 (1971) 319–328.
EPA (Environment Protection Agency, US). Sampling and analysis procedures for screening of industrial effluents for priority pollutants, April 1977.
EPA (Environment Protection Agency, US). Ambient water quality criteria for chlorinated phenols (EPA 440/5–80-032), for 2-chlorophenol (EPA 440/5–80-034), for 2, 4-dichloro-phenol (EPA 440/5–80-042), for pentachlorophenol (EPA 440/5–80-065, 1980a).
Faas L F, J C Moore. Determination of pentachlorophenol in marine biota and sea water by gas-liquid chromatography and high pressure liquid chromatography. J Agric Food Chem 27 (1979) 554–557.
Fogelqvist E, B Josefsson, C Roos. Determination of carboxylic acids and phenols in water by extractive alkylation using pentafluorobenzylation, glass capillary GO and electron capture detection. J High Res Chromatogr 3 (1980) 568–574.
Giger W, C Schaffner. Determination of phenolic water pollutants by glass capillary gas chromatography. In “Advances in the identification and analysis of organic pollutants in water”, 1 H Keith (ed), Ann Arbor Science Publin press (1981).
Grob K, G Grob, K Grob Jr. Deactivation of glass capillary columns by silylation. Part 1. Principles and basic techniques. JHRC & CC 2 (1979) 31–35.
Hattula M L, H Reunanen, V-M Wasenius, R Krees, A U Arstila. Toxicity of 4-chloro-o-cresol to fish. Light microscopy and chemical analysis of the tissue. Bull Environ Contam Toxicol 22 (1979) 508–511.
Jensen S, L Renberg, L Reutergårdh. Residue analysis of sediments and sewage sludge for organochlorines in the presence of elemental sulfur. Anal Chem 49 (1977) 316–318.
Kawahara F K. Gas chromatographic analysis of mercaptans, phenols and organic acids in surface waters with the use of pentafluorobenzyl derivatives. Environ Sci Technol 5 (1971) 235–239.
Keith L H. Analysis of organic water pollutants. Environ Sci Technol 13(1979) 1469–1471.
King W P, K T Joseph, P T Kissinger. Liquid chromatography with amperometric detection for determining phenolic preservatives. JAOAC 63 (1980) 137–142.
Kozak V P, G V Simsiman, G Chesters, D Stensby, J Harkin. Reviews of the environmental effect of pollutants: XI. Chloro-phenols. Oak Ridge Nat Lab ORNL/EIS-128, June 1979 (EPA/600/ 10).
Lindstrom K, J Nordin. Gas chromatography - mass spectrometry of chlorophenols in spent bleach liquors. J Chromatogr 128 (1976) 13–26.
McCallum N K, R J Armstrong. The derivatization of phenols for gas chromatography using electron capture detection. J Chromatogr 78 (1973) 303–307.
Pierce R H, DMVictor. The fate of pentachlorophenol in an aquatic ecosystem in “Pentachlorophenol”, K Ranga Rao (ed), Plenum Publ Corp (1978) 41–51.
Pinkerton K A. Direct LC analysis of selected priority pollutants in water at ppb levels. J of HRC $ CC 4 (1981) 33–34.
Realini P A. Determination of priority pollutant phenol in water by HPLC. J Chromatogr Sci 19 (1981) 124–129.
Renberg L. Ion exchange technique for the determination of chlorinated phenols and phenoxy acids in organic tissue, soil and water. Anal Chem 46 (1974) 459–461.
Renberg L. Gas chromatographic determination of phenols in water samples as their pentafluorobenzoyl derivatives. Chemo-sphere10 (1981a) 767–773.
Renberg L. Gas chromatographic determination of chlorophenols in environmental samples. Natl Swedish Environment Protection Board, report SNV PM 1410 (1981b).
Renberg L, K Lindström. C18-reversed phase trace enrichment of chlorinated phenols, guaiacols and catechols. J Chromatogr 214 (1981) 327–334.
Rodgers I H. Isolation and chemical identification of toxic components of kraft mill wastes. Pulp Pap Mag Can 74 (1973) T303-T308.
Rossum P van, R G Wegg. Isolation of organic water pollutants by XAD resins and carbon. J Chromatogr 150 (1978) 381–392.
Rudling L. Determination of pentachlorophenol in organic tissues and water. Water Res 4 (1979) 533–537.
Shafik T M, H C Sullivan, H R Enos. Multiresidue procedure for halo- and nitrophenols. Measurement of exposure to biodegra dable pesticides yielding these compounds as metabolites. J Agrio Food Chem 21 (1973) 295–298.
Stark Å. Analysis of pentachlorophenol residues in soil, water and fish. J Agrio Food Chem 17 (1969) 871–873.
Supelco Inc, Bellefonte, Pennsylvania 16823, USA. A single capillary column for the separation of priority water pollutants. GC reporter V (September 1980).
Author information
Authors and Affiliations
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 1982 ECSC, EEC, EAEC, Brussels and Luxembourg
About this paper
Cite this paper
Renberg, L. (1982). Determination of Phenolics in the Aquatic Environment. In: Bjørseth, A., Angeletti, G. (eds) Analysis of Organic Micropollutants in Water. Springer, Dordrecht. https://doi.org/10.1007/978-94-009-7804-1_35
Download citation
DOI: https://doi.org/10.1007/978-94-009-7804-1_35
Publisher Name: Springer, Dordrecht
Print ISBN: 978-94-009-7806-5
Online ISBN: 978-94-009-7804-1
eBook Packages: Springer Book Archive