Analytica Chimica Acta 406 (2000) 309–315
Automatic determination of fat in milk by use of a flow injection system
with a piezoelectric detector
Lisbeth Manganiello
a,1
, Angel R´ ıos
a
, Miguel Valcárcel
a,∗
, Angel Ligero
b
, Teresa Tena
c
a
Department of Analytical Chemistry, Faculty of Sciences, University of Córdoba, E-14004 Cordoba, Spain
b
Departament of Physics, Faculty of Sciences, University of Córdoba, E-14004 Cordoba, Spain
c
Departament of Chemistry, University of La Rioja, E-26004 Logroño, Spain
Received 2 June 1999; received in revised form 1 October 1999; accepted 10 October 1999
Abstract
A new method for the direct determination of total fat in milk by use of a quartz crystal microbalance was developed.
The method is based on a (micro) extraction procedure that is carried out in a flow injection system. Samples are diluted
with an ethanol–water mixture and injected into the flow system, where they are mixed with n-hexane in an extraction coil.
The analyte is determined in the organic phase. The calibration thus achieved is linear in the range 0.20–0.45% w/v, and the
relative standard deviation is ±3.2% (n = 11; P = 0.05). The throughput is 12 samples per hour. The proposed method was
used to determine fat matter in milk samples; the results were found to be competitive with those of official methods for the
same purpose. ©2000 Elsevier Science B.V. All rights reserved.
Keywords: Flow system; Piezoelectric detection; Fat; Milk
1. Introduction
The use of the piezoelectric quartz crystal as
microbalance detector was originally conceived by
Bruckenstein and Shay [1], who developed a circuit
that allowed the simultaneous measurement of the in
situ frequency change accompanying electrolysis at
the working electrode as a function of either elec-
trode potential or current. Also, they proposed using
an oscillating quartz crystal as an electrochemical
quartz microbalance. The in situ mass sensitivity of
∗
Corresponding author. Fax: +34-957-218606.
E-mail address: qalmeobj@uco.es (M. Valc´ arcel).
1
Permanent address: Chemical Research Centre, Faculty
of Engineering, University of Carabobo, B´ arbula, Carabobo,
Venezuela.
the crystal as determined by electrodeposition of sil-
ver, is quite consistent with the value predicted from
the Sauerbrey [2] equation. This author also inves-
tigated the effects of the solution temperature and
viscosity, and the thickness of the liquid film on top
of the crystal, and correlated his results with theory.
Subsequently Alder and McCallum [3] reviewed the
theory and applications of piezoelectric crystals for
mass measuring. They concluded that many of the
shortcomings and advantages of piezoelectric crystal
detectors had been identified and that equipment and
data processing had developed to an extent allowing
one to identify appropriate situations for application
of the piezoelectric crystal detector under real-life
conditions. Thus, applications where only a modest
level of selectivity is required (e.g. to monitor fam-
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