Trends in Analytical Chemistry, Vol. 23, No.
3, 2004
Traceability of environmental
chemical measurements
Ph. Quevauviller
The concept of traceability implies that measurement data are linked to
stated references through an unbroken chain of comparisons, all with
stated uncertainties. This paper discusses how traceability can be con-
ceived in the context of environmental measurements, in particular the
various elements of the traceability chain (e.g., SI units, documented
standards, reference materials) to which chemical environmental data
may be linked.
# 2004 Elsevier Ltd. All rights reserved.
Keywords: Documented standards; Environmental measurements; Reference mate-
rials; Stated references; Traceability; Units
1. Introduction
Ph. Quevauviller*
European Commission, DG
Environment (BU9 3/121), rue Environmental chemical measurements
de la Loi 200, B-1049 Brussels, concern a wide range of abiotic matrices
Belgium (e.g., air, water, soil and sediment) and
biological matrices (e.g., plants and biolo-
gical tissues), which are analysed for
their contents that comprise a huge vari-
ety of chemical substances at various
levels of concentrations. The complexity
of the measurements and the increasing
demand for data of demonstrated quality
go hand in hand with fundamental dis-
cussions, a key issue of which is trace-
ability.
The traceability concept is a heritage of
metrology, as it was conceived for physi-
cal measurements (e.g., mass, length,
time and temperature) more than a cen-
tury ago; it is now extensively discussed
in the light of the specicities of chemical
and biological measurements [1,2] and
was recently discussed with regard to
environmental measurements [3,4].
Discussions generally highlight that a
direct application of theoretical metrol-
ogy concepts to environmental measure-
*Tel.: +32 (2) 296-3351;
Fax: +32 (2) 295-8072; ments is impossible, because there are
E-mail: philippe. major dierences between chemical/bio-
quevauviller@cec.eu.int logical and physical measurement pro-
0165-9936/$ - see front matter # 2004 Elsevier Ltd. All rights reserved. doi:10.1016/S0165-9936(04)00314-0
Trends
cesses (e.g., chemical analysis results
often strongly depend upon the nature of
samples, whereas physical measurements
are less or not aected), a wide variety of
analytical problems are encountered in
relation to dierent parameters and
matrices, and necessary preliminary
steps (e.g., sampling and sample pre-
treatment) may aect the nal result
[3]. In this respect, theory seems to be
far removed from practice and real-life
situations, and the traceability concept,
as applied to environmental measure-
ments, is still prone to many mis-
understandings.
To introduce this Special Issue of Trends
in Analytical Chemistry on the traceability
of environmental measurements, this
article recalls the main features that have
already been discussed [3].
2. Denitions
Traceability is dened as the property of
the result of a measurement or the value
of a standard whereby it can be related to
stated references, usually national or
international standards, through an
unbroken chain of comparisons all
having stated uncertainties [5].
In this denition, three key elements
may be distinguished:
1. the link to stated references;
2. the unbroken chain of comparisons;
and,
3. the stated uncertainties.
How these elements apply to chemical
measurements has been, and still is
being, discussed [6^8]. This article exam-
ines how they may be understood in the
context of environmental measurements.
171
Trends
2.1. Stated references
In the ISO (International Standards Organisation) de-
nition [5], the stated references may be reference meth-
ods, reference materials or SI (Syste'me International)
units (kg or mole for chemical measurements) [9]. The
theory implies that all chemical measurements should
aim to be traceable to SI units. In practice, however,
chemical measurements are based on approximations
via comparisons of amounts, instrumental response
generated by a number of particles, etc. In other words,
establishing SI traceability of chemical measurements
implies a demonstration of the extent to which these
approximations are unambiguously related to the
stated references [9]. In the case of environmental
chemical measurements, traceability may, in principle,
be achieved in relation to either a reference material
(pure substance or matrix certied reference material
(CRM)) or to a reference method (e.g., standardised
method). This is discussed below.
2.2. Unbroken chain of comparison
The unbroken chain of comparison implies that no loss
of information should occur during the analytical pro-
cedure (e.g., incomplete recovery or contamination).
The longer and more complex the analytical procedure,
the higher the risks of breaking this chain of compar-
ison, i.e. achieving this requirement is more or less dif-
cult according to the analytical problem under
consideration. It will be more critical for techniques
involving successive analytical steps (e.g., extraction,
separation and detection) and less acute for direct
measurement procedures (e.g., sensors), which may,
however, be faced with other diculties (e.g., lack of
sensitivity or lack of selectivity). Environmental mon-
itoring brings an additional diculty, i.e. sample collec-
tion and sample storage. These two steps form an
integral part of the traceability chain, which is too often
forgotten.
2.3. Stated uncertainties
Aspects related to uncertainties are still often over-
looked by many analysts. In theory, traceability implies
that the uncertainty of all the stated references that
contribute to this measurement is duly considered. This
means, in other words, that uncertainty components
should theoretically be estimated at each step of an ana-
lytical process. It also means that the smaller the chain
of comparison the better the uncertainty of the nal
result. It is obvious that, in practice, and in particular
for complex environmental measurements, the theory
will not be applicable (e.g., the uncertainties of sam-
pling and sample pre-treatment operations are hardly
quantiable). The reader is referred to the specialised
literature on aspects of uncertainty [2,10], which I will
not discussed in this article. Rather, I will focus on the
rst two elements?stated references and unbroken
172 http://www.elsevier.com/locate/trac
Trends in Analytical Chemistry, Vol. 23, No. 3, 2004
chain of comparison?which are more likely to be
prone to misunderstandings.
2.4. Traceability versus accuracy
Traceability should not be confused with accuracy. The
latter covers the terms trueness (closeness of agreement
between the true value and the measured value) and
precision (closeness of agreement between the results
obtained by applying the same experimental procedure
several times under prescribed conditions).
General aspects of quality assurance of environ-
mental measurements (including considerations on
accuracy) have been discussed extensively in the litera-
ture [11,12] and will not be repeated here. One should
remember that a method that is traceable to a stated
reference is not necessarily accurate (i.e. the stated refer-
ence does not necessarily correspond to the true
value), whereas an accurate method is always trace-
able to what is considered to be the best approximation
of the true value (dened as a value, which would be
obtained by measurement, if the quantity could be com-
pletely dened and if all measurement imperfections
could be eliminated [5]).
Another confusion that arises is between precision
and uncertainty, which are often considered similar
concepts; that is incorrect, since uncertainty includes
both random and systematic errors, whereas precision
is linked solely to random errors [6].
Environmental measurements are based on a succes-
sion of actions, namely:
(i) sampling, storage and preservation of repre-
sentative samples;
(ii) pre-treatment of a sample portion for quantita-
tion;
(iii) calibration;
(iv) nal determination; and,
(v) calculation and presentation of results.
Starting from this, let us examine how traceability
may be understood in the context of environmental
measurements.
3. A basic reference: SI units
SI units correspond to fundamental units that are used
in metrology. They establish units of length (metre),
mass (kilogram), time (second), temperature (Kelvin),
etc. The unit that underpins chemical measurements is
the unit of amount of substance, the mole. In principle,
all chemical measurement data should be traceable to
the mole [2]. In practice, however, with the mass stan-
dard, there is no 12C mole standard, and the kg
is used to dene the mole [5]. Therefore, chemical
measurements are actually traceable to the mass unit,
Trends in Analytical Chemistry, Vol. 23, No. 3, 2004
the kg. In other words, environmental chemical mea-
surements are based on the determination of amount of
substance per mass of matrix. One should not confuse
this traceability to mass units with the traceability to
the true value of the substance in the matrix, which and tools, etc. [16,17]. The nature of the sample and of
was discussed in a previous paper [3].
4. Standardised procedures as references
Routine environmental measurements often rely on
standardisation through the elaboration of docu-
mented standards (norms) related to measurement pro-
cedures, which aim to establish minimum quality
requirements and to improve the comparability of ana-
lytical results. Standardised methods may also be linked
to environmental regulations. In the case of measure-
ments based on a standardised procedure, the reference
will be directly related to the documented protocol,
which thus represents one of the links of the traceability
chain. This reference is of particular key importance for
environmental measurements based on the use of oper-
ationally-dened parameters (e.g., extractable trace
elements determined by single or sequential extraction
procedures). Indeed, in this case, the analytical results
are directly linked to the analytical protocol that has to
be strictly followed to ensure a proper comparability of
results [13,14]. In other words, the traceability chain is
broken if the protocol is not strictly followed [3].
Standardised methods (written standards) for envir-
onmental measurements were developed for sampling
and analytical methodologies in the form of docu-
mented protocols that describe in detail the procedures,
from sub-sampling to the actual determination. The use
of standard methods in environmental monitoring
should evolve with the analytical progress in order to
avoid old-fashioned methods linked to regulations that
remain mandatory for legal reasons. This was recog-
nised by standardisation bodies (e.g., ISO and CEN (Eur-
opean Committee for Standardisation)), which now
allow progress in analytical technologies to ow into
standardisation work. One should keep in mind that the
use of a standardised method does not guarantee that
errors will not occur, i.e. such methods provide only an
analytical framework that is considered as the refer-
ence for a given measurement. There are examples of
operationally-dened procedures used for soil and sedi-
ment analyses in the literature [13,14], and they were
discussed in a previous paper [3]. This aspect is also
described elsewhere in this Special Issue [15].
Detailed (documented) guidelines have also been
developed for sample collection and storage, albeit they
are more dicult to set up; however, they remain the
primary source of error in environmental measure-
ments, and hence one of the weakest links of the trace-
ability chain.
Trends
Sampling standards generally dene the sampling
method, the number of samples to be collected, their
representation, the frequency of sampling (taking into
account natural variations), the sampling techniques
the substance to be monitored dictate the choice of the
sampling, which therefore has to be adapted case by
case [3]. Recommendations are available in the scien-
tic literature [18,19], but there are very few examples
of documented standards that can formally be used as
stated references for environmental measurements.
Noteworthy progress has been made in the eld of
soil monitoring through a systematic interlaboratory
evaluation of sampling and sample pre-treatment
procedures [20]; more recently, a systematic study
was performed to evaluate the variability of results
attributable to sampling for groundwater analysis
[21].
A similar situation to that in sampling is encountered
in sample storage, for which guidelines and recommen-
dations are available with regard to protection of the
samples from light and elevated temperatures. Much
remains to be done for systematic evaluation of the var-
ious sampling and sample pre-treatment guidelines,
which should preferably be standardised at interna-
tional level to ensure that clear references may be used
to improve data comparability of environmental
measurements.
5. Reference methods
Analytical methods will dier in the link between the
signal produced by a given determined substance and
the signal obtained from the calibration material. In the
case of the majority of environmental measurements,
this link usually relates to an amount of substance of
established purity and stoichiometry. Complex envir-
onmental measurements (e.g., related to chemical spe-
cies of elements or trace organic pollutants) are based
on successive analytical steps, such as extraction, deri-
vatisation, separation and detection. This stepwise ana-
lysis multiplies the risk that the traceability chain is
broken because of a lack of proper tools (e.g., reference
materials (see Section 6), secondary standards, etc.),
which are required to evaluate, for example, extraction
recoveries, derivatisation yields, etc. [3,8]. For other
methods (e.g., XRF (X-ray uorescence spectroscopy)),
the basic links comprise CRMs (see Section 6).
With respect to reference methods, so-called primary
methods certainly represent a cornerstone for achiev-
ing traceability: these methods have the highest metro-
logical qualities; their uncertainty can be established in
terms of SI units; the analytical results can be accepted
without reference to an external calibrating material;
they have few random errors; and, they are supposed to
http://www.elsevier.com/locate/trac 173
Trends
be exempt from systematic errors [1,5]. Using primary
methods guarantees, in principle, that measurements
will be traceable to SI units, i.e. traceability links will be
established to the true value of the amount of the
substance. Unfortunately, primary methods mainly
exist only for trace-element determinations. In the case
of determinations of trace organic and organometallic
compounds, the analysis generally relies on an extrac-
tion step, for which recoveries can hardly be demon-
strated at this stage using primary methods (unless
CRMs containing compounds involved may be used for
this purpose). Indeed, the traceability chain will be bro-
ken at several stages and the stated references will rely
only on approximations (recovery estimates). The
better these approximations are, the closer the trace-
ability of the measurement to the true value. In the
cases of trace organic and organometallic determina-
tions in environmental matrices, primary methods do
not exist, since there are no means at present to give
proof that extraction or chemical reactions (e.g., deri-
vatisation) have yielded a 100% recovery.
An example of frequently used primary method in
environmental chemistry is isotope dilution coupled
with mass spectrometry (IDMS) or inductively
coupled plasma mass spectrometry (ID-ICPMS). This
method is increasingly used for environmental studies,
as illustrated in the present issue [22,23]. It was argued
that the nal ID-based results are actually traceable to
the true value of organic or organometallic com-
pounds in extracts of the analysed environmental
samples but not necessarily to the true value in the
sample, because the link to extraction recovery
hampers this traceability [3]. Progress is therefore
needed in this eld to improve this particular link of the
traceability chain.
Methods that are based on internal or external cali-
bration rely on the availability of calibrants of high
purity and veried stoichiometry, which represents the
last link of the traceability chain (i.e. calibration of
the detector signal). Traceability of environmental
measurements requires that, in principle, all the steps
of an analytical technique be recorded in such a way
that the result of the nal determination is linked
through an unbroken chain of comparisons to appro-
priate standards. In other words, rmly establishing the
traceability of chemical measurements means that sev-
eral primary chemical reference materials in the
form of (ultra-)pure substances are interlinked by well-
known, quantitative, high-precision high-accuracy
chemical reactions [24]. In practice, this is not achiev-
able for the vast majority of environmental measure-
ments since, as discussed above, there are many weak
links in the traceability chain (e.g., extraction in rela-
tion to recovery estimates, derivation owing to a lack of
appropriate secondary calibrants, etc.) [3]. In other
words, many environmental measurement methods
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Trends in Analytical Chemistry, Vol. 23, No. 3, 2004
depend on a number of more or less well-controlled
parameters that may vary from one sample to another.
As stressed Section 7, analytical steps that rely on a
recovery estimate can be validated only by comparison
with independent methods, giving a good indication on
data comparability but not necessarily on accuracy.
Hence, few of these methods may be considered as refer-
ence methods unless they are documented with a full
description of all the analytical operations and the
limits of applicability of the method [3], which is, for
example, the case of ocial methods that are
required in some environmental regulations.
6. Reference materials
The role and the use of reference materials are well
known, in principle. They are either CRMs, which are
used as calibration materials (pure substances or solu-
tions, or materials of known composition for techniques
requiring matrix-matched calibrants (e.g., XRF) or
matrix materials representing as far as possible real
matrices for the verication of the measurement pro-
cess, or (not certied) laboratory reference materials
(LRMs, also known as quality control (QC) materials),
which are used, for example, for interlaboratory studies
or internal QC (control charts). Details of the types, the
roles and the uses of CRMs and LRMs as applied to
environmental measurements are available in the lit-
erature [12].
Control charts [25], which are used to monitor the
reproducibility of methods (based on the repetition of
analysis of one or several reference materials) may be
considered as long-term stated references for analytical
measurements, since they allow the monitoring of ana-
lytical variations according to an anchorage point, i.e.
the reference material(s). This is a mean to check the
method reproducibility but not necessarily the trueness
of the measurements. For such verication, ocial cer-
tifying organisations attempt, wherever possible, to
produce reference materials estimating the true values
as closely as possible, which, in the case of matrix envir-
onmental CRMs, is achieved mainly by employing a
variety of methods with dierent measurement princi-
ples in the material certication study. A good agree-
ment among the various methods used enables the
assumption (but not the rm demonstration) that no
systematic error was left undetected, and that the refer-
ence (certied) values are the closest estimate to the
true value. Wherever possible, this approach should
include primary methods (see above), which seldom
exist for analyses involving an extraction or a derivati-
sation step. In many instances, the use of various meth-
ods enables analysts to obtain consensus values that
are accepted as true values (reecting the state-of-the-
art and hence ensuring data comparability).
Trends in Analytical Chemistry, Vol. 23, No. 3, 2004
Some CRMs are intended for calibration purposes. In
such a case, the uncertainty of the certied value is of
prime importance, since it will aect the nal uncer-
tainty of the measured value in the unknown sample.
In the case of certied pure substances or calibrating
solutions, the uncertainties of certied values are
usually negligible in comparison with the method
uncertainty, which is not the case with matrix CRMs
that are, in principle, reserved for the validation of
methods. In specic cases, matrix CRMs are used for
calibration purposes, for example, for non-destructive
methods (e.g., XRF); however, the larger uncertainty of
the certied values may lead to too large an uncertainty
in the nal results (thus leading to semi-quantitative
measurements).
In the case of environmental measurements, the wide
variety of matrices and substances encountered, in
principle implies that a large range of matrix reference
materials representative from various sample types
(e.g., sediments, soils, plants, waters and biological tis-
sues) should be available. However, the best match
between a CRM and a natural sample can never be
achieved and compromises are necessary in most
instances. An example of matrix CRMs that simulate
environmental samples is described in this issue (for
wastewater reference materials) [26]. As discussed pre-
viously [3,4], reference materials represent physical
stated references to which measurements can be linked
but which call for a cautious evaluation resulting from
matrix dierences. It was stressed that a correct result
obtained with a matrix CRM does not give a full assur-
ance that correct results will be achieved when ana-
lysing unknown samples, because of dierences in
matrix composition [8].
The traceability of environmental measurements on
the basis of matrix CRMs (representing complex chemi-
cal systems) to SI units is largely debated [3]. This is
illustrated by the various contributions to this special
issue, in particular that by Charlet and Marschal [27].
As discussed above, this results from the lack of cer-
tainty that the certied values will correspond to true
values, in particular with regard to complex matrix
reference materials analysed for their contents (e.g., of
trace organic or organometallic compounds). This does
not diminish the value of the CRMs, since the con-
sensus values play the role of reference in achieving
traceability for a given environmental measurement,
(linking results to a wide analytical community and
thus ensuring data comparability) but do not necessa-
rily allow trueness to be checked.
In addition, there are many environmental analytical
elds for which CRMs are lacking (or are available but
with a matrix too far removed from the analysed sam-
ples) or cannot be prepared because they are unstable
[3]. In these cases, other approaches have to be
followed to achieve traceability (e.g., interlaboratory
Trends
studies, see Section 7). Where there is good corres-
pondence between the matrix of samples and the
matrix of CRMs, this reference is certainly the most
appropriate one for checking the accuracy of analytical
methods and comparing the performance of one
method with other methods (or other laboratories).
Similar comments with respect to representativeness
may be made concerning matrix LRMs used for inter-
nal QC purposes (establishment of control charts).
Further discussions on traceability links represented by
reference materials are available in the literature
[3,4,28].
7. Prociency testing (PT)
In principle, PT enables laboratories to establish exter-
nal references for evaluating the performance of their
methods. In this framework, one or more reference
materials are distributed by a central organisation to
several laboratories for the determination of given sub-
stances. Comparing laboratory results (based on dier-
ent methods) allows the detection of possible sources of
errors linked to a specic procedure or related to the
way a method was applied by a given laboratory. When
the testing focuses on a single method, this enables per-
formance criteria (e.g., precision) to be checked. The
references (establishing the traceability link) are again
based on reference materials that have to follow the
usual requirements. However, by contrast with refer-
ence materials used for internal QC, PT may involve
samples with a limited shelf life, which may be dis-
tributed to laboratories for analysis of particular para-
meters that could not be evaluated using stabilised
RMs. Examples are fresh materials with a short-term
preservation period [3]. An example of PT is quoted in
this issue [27]. PT may also be based on reference sites
(e.g., to evaluate sampling procedures (as mentioned
above for soil analyses [20]) or a bulk common sample
to be analysed by the laboratories at the same time (e.g.,
a tank full of seawater for microbiological measure-
ments)).
As discussed above for RMs, the measurement
values obtained in the framework of interlaboratory
studies (using dierent techniques) may be considered
as an anchorage point representing the analytical
state-of-the-art; this oers laboratories a means to
achieve comparability (i.e. traceability) of their results
to a recognised reference, which in this case is a
consensus value (generally the mean of laboratory
means). Let us stress again that this reference does not
enable traceability to the true value of the substance
in the medium to be achieved, but it represents a very
useful method for achieving comparability of environ-
mental measurements using an external QC scheme
[3].
http://www.elsevier.com/locate/trac 175
Trends
8. Environmental specimens: a long-term
reference
Another type of reference that is used in environmental
studies relies on specimen banking [29,30]. In this
approach, environmental samples are collected, pro-
cessed and stored under conditions that prevent any
signicant changes of their chemical composition [29].
This enables development of a systematic repository of
environmental samples, which may later provide infor-
mation about pollution levels and tools for evaluating
contamination trends.
Specimen banking may be considered the best refer-
ence system for long-term environmental monitoring
[3]. Indeed, besides the specimens that are true
stated references of the environment status at the time,
stabilised reference materials (i.e. in dried form) can
also be produced from surplus specimen material in
order to monitor the reproducibility of analytical tech-
niques, hence ensuring internal QC uses the most repre-
sentative samples [29]. Fresh reference materials
may also be prepared and used for the development and
optimisation of analytical procedures, internal QC and
stability experiments with environmental specimens
[30]. In other words, the long-term storage of environ-
mental specimens serves the purpose of monitoring
temporal and spatial contamination trends. These spe-
cimens, taken as stated references, also enable analyses
to be repeated, focusing on specic contamination stud-
ies when more sophisticated (accurate) analytical
methods become available. This approach is further dis-
cussed in the literature [3,29,30].
9. Conclusions
Environmental studies and monitoring based on chemi-
cal measurements can only be valid if data are obtained
under a reliable quality assurance regime. A manda-
tory requirement is the comparability of data (e.g., for
evaluating spatial and temporal contamination
trends). This requires the demonstration of data trace-
ability to stated references as extensively discussed in
the present issue.
Case studies examining the traceability chain for
environmental measurements of increasing complexity
(starting from trace elements in water to organome-
tallic compounds in solid matrices) have been discussed
in previous papers [3,4]. This general introductory
article has recalled the main features of traceability, as
they apply to environmental measurements.
As a general conclusion, the confusion between
traceability to well-dened, accepted references and
accuracy should be avoided. The rst concept is a
changing feature (i.e. stated references may evolve with
progress of knowledge and of technical capabilities,
176 http://www.elsevier.com/locate/trac
Trends in Analytical Chemistry, Vol. 23, No. 3, 2004
while still maintaining comparability of data), but it
does not necessarily mean that the produced data are
accurate (i.e. close to true value). In other words,
environmental measurements may be traceable to
pure calibrating substances, CRMs or documented
standards, the two latter often corresponding to con-
sensus values and not true values [3,4]. Demon-
strating traceability of an amount of substance to its
true value in a given medium is, therefore, hardly ever
achievable in practice and compromises have to be
found in relation to the best state-of-the-art in analysis.
Progress remains necessary to ensure that references
used in environmental chemistry (in particular the
reference materials) will, without any ambiguity, allow
accuracy to be achieved on the basis of (certied) values
being closer and closer to the true values. Only this pro-
gress will enable accuracy of environmental measure-
ments to be rmly demonstrated, so that traceability of
these measurements to the true amounts of con-
taminants in the environment will be achievable.
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