Short Communication
Micro versus macro solid phase extraction for monitoring water
contaminants: A preliminary study using trihalomethanes
Lydon D. Alexandrou
a
, Michelle J.S. Spencer
b
, Paul D. Morrison
a
, Barry J. Meehan
b
, Oliver A.H. Jones
a,
⁎
a
Australian Centre for Research on Separation Science (ACROSS), School of Applied Sciences, RMIT University, GPO Box 2476, Melbourne, VIC 3001, Australia
b
School of Applied Sciences, RMIT University, GPO Box 2476, Melbourne, VIC 3001, Australia
HIGHLIGHTS
• Traditional and micro solid phase extraction methods were compared.
• Four common disinfection by products were used to assess each method.
• Micro SPE provided better recoveries for all compounds tested than traditional SPE.
• Micro SPE required less sample and less solvent volumes than traditional SPE.
• Micro SPE is underexploited but has a large range of potential application in environmental science.
abstract article info
Article history:
Received 30 October 2014
Received in revised form 19 January 2015
Accepted 19 January 2015
Available online 24 January 2015
Editor: D. Barcelo
Keywords:
Trihalomethanes
Electron capture detection
Micro solid phase extraction
Water
Solid phase extraction is one of the most commonly used pre-concentration and cleanup steps in environmental
science. However, traditional methods need electrically powered pumps, can use large volumes of solvent
(if multiple samples are run), and require several hours to filter a sample. Additionally, if the cartridge is open
to the air volatile compounds may be lost and sample integrity compromised. In contrast, micro cartridge
based solid phase extraction can be completed in less than 2 min by hand, uses only microlitres of solvent and
provides comparable concentration factors to established methods. It is also an enclosed system so volatile com-
ponents are not lost. The sample can also be eluted directly into a detector (e.g. a mass spectrometer) if required.
However, the technology is new and has not been much used for environmental analysis. In this study we com-
pare traditional (macro) and the new micro solid phase extraction for the analysis of four common volatile tri-
halomethanes (trichloromethane, bromodichloromethane, dibromochloromethane and tribromomethane).
The results demonstrate that micro solid phase extraction is faster and cheaper than traditional methods with
similar recovery rates for the target compounds. This method shows potential for further development in a
range of applications.
© 2015 Elsevier B.V. All rights reserved.
1. Introduction
Solid phase extraction (SPE) is a simple and effective extraction
technique for isolating target compounds from aqueous solutions. It uti-
lises a small cartridge packed with solid particle, chromatographic ma-
terial (sorbent or resin) that acts much like a high performance liquid
chromatography (HPLC) phase and which utilises partitioning or
distribution processes to chemically separate the different components
of a liquid sample (Huck and Bonn, 2000).
SPE was developed in the late 1970s and has been in common use
since the mid-1980s (Huck and Bonn, 2000). Since that time it has be-
come one of the most powerful and commonly used sample preparation
techniques in analytical and environmental chemistry. It enables
researchers to isolate organic analytes from large volumes of water, con-
centrates trace amounts of contaminants to detectable levels and elim-
inates much of the glassware and organic solvents necessary with
liquid–liquid extraction procedures (Jones et al., 2003). Additionally,
by switching from the original environmental matrix to an organic sol-
vent, or ultra pure water, the final analysis is simplified and the demand
placed on analytical instrumentation is substantially reduced (Thurman
and Mills, 1998).
Traditional, cartridge based systems do have some limitations. Pre-
concentration of trace levels may require the filtration of large volumes
Science of the Total Environment 512–513 (2015) 210–214
Abbreviations: SPE, Solid phase extraction; THMs, Trihalomethanes; DBP, Disinfection by-
product; HPLC, High-performance liquid chromatography; HAAs, Haloacetic acids; HANs,
Haloacetonitriles; HAs, Haloacetaldehydes; HKs, Haloketones; TCM, Trichloromethane;
BDCM, Bromodichloromethane; DBCM, Dibromochloromethane; TBM, Tribromomethane;
WWTP, Wastewater treatment plant; μECD, Micro-electron capture detector; LLE,
Liquid–liquid extraction
⁎ Corresponding author.
E-mail address: Oliver.Jones@rmit.edu.au (O.A.H. Jones).
http://dx.doi.org/10.1016/j.scitotenv.2015.01.057
0048-9697/© 2015 Elsevier B.V. All rights reserved.
Contents lists available at ScienceDirect
Science of the Total Environment
journal homepage: www.elsevier.com/locate/scitotenv