Food Control 17 (2006) 719–726

www.elsevier.com/locate/foodcont

Quality assurance of volumetric glassware for the determination

of vitamins in food
a,*
I. Castanheira , E. Batista b, A. Valente a, G. Dias a, M. Mora b, L. Pinto b, H.S. Costa a

a
Department of Food Safety and Nutrition, National Institute of Health Dr. Ricardo Jorge, Av. Padre Cruz, 1649-016 Lisboa, Portugal
b
Central Metrology Laboratory, Portuguese Institute for Quality Rua António Gião, 2 Caparica, Portugal

Received 2 December 2004; received in revised form 7 April 2005; accepted 11 April 2005

Abstract

Volumetric measurements are currently used in the analytical process to determine the vitamins content in foods. The variations
in stability and integrity of volumetric apparatus, although relatively small when compared with other sources of error, should be
monitored. The main purpose of this study was to investigate and identify a number of variables which, in daily use, can affect the
life cycle of volumetric glassware. The role of in-house metrological hierarchy, the operatorÕs performance and the effect of temper-
ature was evaluated for single volume flasks, single- and multi-mark pipettes. Biased nominal capacity was applied in the calculation
of water-soluble vitamins (B1, B2, B6, niacin) and fat-soluble vitamins (A, D, E) content. Persistent bias due to volumetric glass-
ware, can reach 11%, in the results obtained for different vitamins content. The largest bias was observed for vitamin B1, perhaps
due to the high amount of volumetric glassware used in the analytical procedure. This is an indication that the cost–benefit of a
calibration plan should be evaluated in a rational way. The regular checking of volumetric glassware for stability and integrity is
discussed on the light of the latest revision of ISO 17025.
Ó 2005 Elsevier Ltd. All rights reserved.

Keywords: Volumetric glassware; Bias; Vitamins; Food; Metrology in chemistry

1. Introduction now explicitly requested in guidelines dealing with food

Quality assurance of volumetric glassware is a rele-
vant step of the food analytical process (Anglov, Peter-
sen, & Kristiansen, 1999; Wood, Nilsson, & Wallin,
1998), and there are cases where volumetric methods
are adopted as CEN methods: Foodstuffs––Determina-
tion of vitamins by high performance liquid chromatog-
raphy (HPLC), (EN 12821; EN 12822; EN 14164; EN
14152; EN 12823-1; EN 14122; CEN/TC 275/WG 9).
Calibrated glassware and traceability to SI units is
*
Corresponding author. Tel.: +351 21 751 93 17; fax: +351 21 752
6400.
E-mail address: isabel.castanheira@insa.min-saude.pt (I. Castan-
heira).
measurements (Codex, 2002; EURACHEM, 2000).
The quality criteria of volumetric glassware has been
studied in recent decades and granted through the use of
metrological procedures, supported on traceability of
nominal value and its confidence interval. ISO (ISO
835/1; ISO 4787) in the early 1980s published a series
of standards where the concept of tolerance limits based
on repeatability of the calibration procedure was intro-
duced. Studies on stability of volumetric glassware were
described later in the 1980s by Burfield and Hefter
(1987). These concepts have recently been reviewed in
the literature (EURACHEM, 2000; Kadis, 2004): The
tolerance limits are calculated in compliance with the
Guide ‘‘Quantifying Uncertainty in Analytical Measure-
ment’’, issued by EURACHEM/CITAC (2000); volu-
metric glassware is considered appropriate if the

0956-7135/$ - see front matter Ó 2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.foodcont.2005.04.010
720 I. Castanheira et al. / Food Control 17 (2006) 719–726
nominal capacity value and its associated uncertainty re-
main within acceptable limits. In the case of volumetric
glassware used in daily measurement practice, the expiry
date of the calibration result, calibration plans and
calibration intervals are defined by the laboratory and
usually operation conditions are not mentioned.
However, this procedure tends to change in the future
due to improved actions introduced by accreditation
bodies, as consensus exists, in the revision of ISO/IEC
17025 to include regular checking of equipment for
stability and integrity (FDIS ISO 17025, 2004).
Confidence in the whole life cycle of the measurement
equipment, from its design to use, framed by metrolog-
ical parameters is a thematic area that has received
much attention in the field of legal metrology. Substan-
tial information on this area exists in OIML D 20
(1988), OIML D 27 (2001), Vaz, Castanheira, Fino,
and Van der Veen (2000), Sommer, Chappell, and
Kochsiek (2001). The equipment is considered appropri-
ate during the time in which deviation from the true
value remains under acceptable limits. The checking
intervals for the equipment in place are designated as
a periodic verification, and the decisions on equipment
performance are based on maximum permissible errors,
as described in OIML recommendation.
This work is a three-step procedure dealing with
monitoring of volumetric glassware used in the measure-
ment of vitamins content in food in compliance with the
latest revision of ISO 17025 (FDIS ISO 17025, 2004). In
the first step, an approach to establish in-house metro-
logical hierarchy is discussed. The identification of crit-
ical parameters in the calibration procedure is presented
in the second step. Finally, in the third step, the impact
of systematic error due to volumetric glassware in the
measurement of vitamins B1, B2, B6, niacin, A, D and
E content was estimated.
2. Materials and methods
2.1. Metrological qualification of volumetric glassware
2.1.1. Metrological hierarchy for volumetric glassware
Laboratory glassware was classified according to its
metrological grade. This was based on an established
hierarchy of traceability chain to SI units through na-
tional standards of measurements and framed by stan-
dard definitions adopted by the International
Vocabulary of Metrology (VIM) (BIPM, 1993). The fol-
lowing Reference Standards Volumetric Glassware
(RSVG) were calibrated at the National Metrology
Institute (NMI): burettes, pipettes, flasks and cylinders
with capacities in the range of 5–500 ml, and stored
under appropriate conditions.
Working Standards Volumetric Glassware (WSVG)
(pipettes of 2 ml and 5 ml; flasks of 20 ml and 50 ml) were
calibrated against reference standards at a Food Analy-
sis Laboratory (FAL) using an appropriate protocol.
The nominal value of volumetric glassware, routinely
used in food analysis, was checked against the assigned
value of the working standard. A set of three or five
20 ml and 50 ml flasks and 1 ml, 2 ml and 5 ml pipettes
currently used in vitamin content determinations were
submitted to several tests described below.
2.1.2. Metrological criteria
Class A volumetric glassware was calibrated at the
NMI and calibration results issued by the NMI were
analysed in terms of the assigned value and associated
uncertainty. The acceptance criterion was defined
according to ISO 4787 (1984). Compliance of the as-
signed value with the acceptance criteria is defined by
Eq. (1) and it was evaluated on the basis of accepted
or rejected.
jxn  xr j
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi < TL ð1Þ
U 2n þ U 2a
where xn is the nominal value, xr is the reference value,
Un is the uncertainty of the nominal value, Ua is the
uncertainty of the assigned value and TL tolerance
limits defined in ISO 1042 and ISO 835.
Volumetric glassware was accepted as reference stan-
dard, when the assigned value and associated uncertainty
were within the acceptance limits. The glassware was des-
ignated as WSVG when the assigned value plus or minus
the associated uncertainty lies outside one of the accep-
tance limits. The glassware was rejected as RSVG, when
the assigned value and associated uncertainty did not fall
in the previous judgement of compliance. In order to
provide confidence of measurements, a calibration pro-
gramme was developed and RSVG were calibrated once
a year by the NMI. The calibration results for time zero,
years two and four were compared with the maximum
acceptable deviation defined by Eq. (1), and used to
establish the external calibration intervals.
2.2. Calibration procedure
2.2.1. Traceability
The in-house calibration hierarchy used to achieve
traceability to SI units was composed of: RSVG, WSVG
and volumetric glassware. The reference value of capac-
ity was obtained by a gravimetric process at the NMI,
according to ISO 4787 (1984), ISO 835 (1981) and ISO
1042 (1998). This was achieved applying a weighing pro-
cedure consisting of 10 weighing cycles, where in each
cycle, the mass corresponding to volume capacity was
obtained by the difference between the filled vessel with
distilled water and the empty vessel. The equation of
proportionality that converts the average mass to
volume measurement is described as:
 I. Castanheira et al. / Food Control 17 (2006) 719–726 721
   
1 q scribed above. The ‘‘blind’’ test was carried out by an
V 20 ¼ ðI L  I E Þ   1 A
qw  qA qB analyst with less experience in the calibration procedure,
 ð1  cðt  20ÞÞ ð2Þ and consisted on the evaluation of results at the gradu-
ation line under study, taking into account three param-
where V20 is the volume at 20 °C (reference tempera- eters: (a) reported value and associated uncertainty; (b)
ture), in ml; IL and IE, the weight of the vessel with water precision and (c) meniscus reading. The ‘‘blind’’ results
and of the empty vessel, respectively, in g; qw, the den- were benchmarked to the ones given by a NMI operator
sity of water, at calibration temperature, in g ml1; qA and adequate statistical tests were applied. The criteria
and qB, the density of air and of the mass pieces, in used to classify the operatorÕs performance were: poor
g ml1 (reference values of 0.0012 g ml1 and 8.0 g ml1, and good performance. This was derived from the sum
respectively); c, the coefficient of cubic thermal expan- of the overall results. Each analyst result was consid-
sion of the material, in °C1 and t, the temperature of ered: satisfactory; questionable or unsatisfactory, if the
the water used in the calibration, in °C. value was respectively, below, equal or above the tabu-
lated value of the statistical test. The operatorÕs perfor-
2.2.2. Measurement uncertainty mance was considered as good, if 75% of the values of
The uncertainty of the glassware calibration process the overall result were satisfactory. The remaining situ-
is defined as a parameter associated with the result of ations were considered as poor performance. This proce-
a measurement that characterizes the dispersion of the dure was applied to two types of volumetric glassware:
values that could be attributed to the measurand, pipettes and flasks of different capacities.
according to EURACHEM Guide (2000). The expres-
sion for the combined standard uncertainty (u(V20)) 2.4. Temperature conditions
was developed from Eq. (2) using the error propagation
formula. The major contributions to the combined stan- The effect of temperature on the nominal capacity
dard uncertainty were estimated through a function of volumetric glassware was carried out at NMI follow-
model, presented in Eq. (3), and considering seven build- ing a three step experimental protocol: first, the glass-
ing blocks: repeatability mass; meniscus; water density; ware was calibrated according to the calibration
temperature; air density; density of mass species and procedure described above; secondly, the glassware
thermal expansion of the material. The expanded uncer- was submitted to a chosen temperature during a period
tainty (U) defined ‘‘as an interval within which the value of time and in the third step, the glassware was equili-
of the measurand is believed to lie with a particular level brated at standard reference temperature and then sub-
of confidence’’ EURACHEM (2000) was calculated mitted to the calibration procedure again. The effect of
using a coverage factor of k = 2, considering 95% as temperature is given by the difference between the vol-
approximate level of confidence. ume at graduation line obtained in the first and third
" 2  2 step.
oV 20 oV 20 Pipettes and flasks were withdrawn from daily rou-
uðV 20 Þ ¼ u2 ðmÞ þ u2 ðqw Þ
om oqw tine laboratory work, divided into three different groups
 2  2 and submitted to this procedure. In group I, the glass-
oV 20 oV 20
þ u2 ðqA Þ þ u2 ðqB Þ ware was submitted daily to a temperature of 4 °C dur-
oqA oqB ing five days (120 h). In group II, the temperature was
 2  2 #12
oV 20 oV 20 set daily (24 h) to 50 °C during five days and the calibra-
2 2 2
þ u ðcÞ þ u ðtÞ þ u ðdV men Þ tion procedure was performed at day one, three and five.
oc ot
In group III, the glassware was maintained during five
ð3Þ days at 50 °C and submitted to the calibration proce-
dure at day five.
where u(m) is the uncertainty of the weighing; u(qw), the
uncertainty of water density; u(qA), the uncertainty of air 2.5. Testing for persistent bias
density; u(qB), the uncertainty of the mass pieces; u(c),
the uncertainty of the coefficient of cubic thermal expan- 2.5.1. Determination of vitamin content
sion of the material; u(t), the uncertainty of the temper- Vitamin determination was done by conventional
ature and u(dVmen), the uncertainty of the meniscus. methodology. This consisted on saponification for fat-
soluble vitamins and hydrolysis for water-soluble vita-
2.3. Operator’s performance mins, followed by liquid–liquid extraction and HPLC
analysis according to the methods described in the liter-
The influence of the operatorÕs performance on the ature: Vitamins A (EN 12823-1), D (EN 12821), E (EN
capacity value of WSVG was evaluated through a cali- 12822) and vitamins B1 (EN 14122), B2 (EN 14152), B6
bration test, using the same experimental procedure de- (EN 14164), niacin (CEN/TC 275/WG 9).
722 I. Castanheira et al. / Food Control 17 (2006) 719–726

2.5.2. Bias due to volumetric glassware

The potential bias of the analytical procedure, due to
laboratory volumetric glassware was studied using two
protocols (A) and (B), and assuming that no other
variation occurred in the measuring system during the
determination of vitamin content. In protocol (A), mea-
surement results were obtained according to standard
operation procedure. In protocol (B) and for each step
of the analytical procedure, the ‘‘nominal value’’ of
volumetric glassware was estimated by adding to the
reference value, the worst value within experimental
variability for the operator and temperature tests. Bias
was considered significant, if the relative difference
between protocol (A) and (B) was larger than the
expanded uncertainty of this difference.

2.6. Statistical analysis

Fig. 1. Calibration results of volumetric glassware as reference
HPLC response characteristics were estimated standards.
through calibration functions obtained by least-squares
regression analysis. The following parameters were con-
sidered: polynomial coefficients and their uncertainties, Reference standard
residuals and regression coefficients. Mean and standard Working standard
deviations of analytical data for vitamins content were UAL
calculated for a significance level of P < 0.05.
The following statistical tests were applied for data
analysis: F-test was used to compare variances of the
replicate analysis, En-score was used to compare two
independent means with the same number of observa- xr
tions and single outlier selection was done by DixonÕs
test (Miller & Miller, 1988).

3. Results and discussion LAL

An overview of calibration results for RSVG is given

in Fig. 1. It can be seen that for different types of
volumetric glassware, the percentage of glassware cali-
brated that failed the acceptance criteria varied from
0% up to 40%. Cylinders are in agreement with the
acceptance criteria defined above; 10% of the flasks cal-
ibrated do not fulfill this criterion; 20% of burettes can-
not be labeled as reference standards and for pipettes,
40% of the candidate standards were not compliant with
the specifications of the acceptance criteria as reference
standards (BIPM, 1993). Calibration results issued for
pipettes as RSVG are presented graphically in Fig. 2,
for time zero, year two and four, revealing that appro-
priate care of volumetric glassware was taken. The same
graphic profile was obtained for flasks. These results,
indicating that nominal capacity remained constant
overtime is probably due to consistent storing and clean-
ing conditions as described by accreditation bodies
(UKAS, 2002). For working standards more than 90%
of pipettes and flasks passed the defined acceptance
criteria.
0 2 4
Time (years)
Fig. 2. Examples of calibration results with reference value and
associated uncertainty: xr, reference value; UAL, upper acceptable
limit; LAL, lower acceptable limit.
An indirect calibration procedure (Rodrı́guez, Gra-
cia, López, & Sánchez, 2001) which consists on the con-
version of the mass into volume and comparison of the
deliverable water of RSVG and WSVG, on a periodi-
cally time schedule of six months and under the assump-
tion that measurement uncertainty remains constant,
was also used.
The establishment of in-house metrological hierarchy
based on an indirect calibration procedure of WSVG,
with more rigorous specifications than the manufacture
tolerances, allows regular checking of volumetric glass-
ware for stability and integrity of daily used glassware
 I. Castanheira et al. / Food Control 17 (2006) 719–726 723

without lost of traceability links. This procedure is more

advantageous than to refer all volumetric glassware to
an external link (European Commission, 1998; EURA-
CHEM, 2003).
Evaluation of the measurement uncertainty, in the
calibration procedure of reference standards, was based
on a model which consists on the contribution of several
standard uncertainties, quantified in terms of experi-
mental standard deviation times the sensitivity coeffi-
cient of each source, as described in Eq. 3. This
empirical model was evaluated by the Ishikawa (1976)
diagram and based on type A (experimental) and type
B (estimated) uncertainties inputs which combines
intralaboratory repeatability and reproducibility with
parameters (e.g.: water density; thermal expansion coef-
ficient) whose contributions derive from tabulated
values published in the literature (Spieweck & Bettin, Fig. 3. Schematic representation of sources and main components of
1992). All the values obtained for the expanded uncer- measurement uncertainty, for the calibration procedure, performed
against national standards.
tainty were below the predicted uncertainties of 0.1%;
0.2%; 0.3% (UKAS, 2002). The values of reference
standards were well within the variation claimed by
the manufacture (Noack, 1998) and in agreement with provided by AFAL are different from the assigned value
the results of Euromet intercomparisons (Euromet, (Armishaw, King, & Millar, 2003). The analystÕs preci-
2004). The uncertainty budget provides a mean to com- sion (ANMI versus AFAL) was evaluated using F-test
pare different contributions to the combined standard and the results were compared with the tabulated values
uncertainty (Fig. 3). The largest contribution came from (Miller & Miller, 1988) demonstrating that AFAL has
experimental sources: mass determination, meniscus been working with a different level of precision. The
reading, temperature, precision of each determination evaluation of operatorÕs performance was grounded on
which includes the operatorÕs performance and which a measurement theory (Mari, 2003), implemented with
was found to be the highest source. Therefore, the oper- two kinds of tests: pair comparison and magnitude esti-
atorÕs performance was accounted for and was subject to mation using a set of reference values in all points of
a more detailed study. scale (Rossi, Crenna, & Codda, 2003). The judgement
The acceptable operatorÕs performance was evaluated of evaluation occurs in three steps: (a) single measure-
applying appropriate statistical tests to identify the main ment through outliers tests; (b) error propagation due
causes of error. Table 1 summarizes the results obtained to statistical evaluation of mean of results (c) estimation
by analysts from the National Metrology Institute degree of inaccuracy by null hypothesis. This approach
(ANMI) and from a Food Analysis Laboratory (AFAL) seems to be very useful to evaluate the analyst skills,
for flasks and pipettes, and for the same calibration pro- to identify the cause of error and to decide on further
cedure. Outliers were not found when DixonÕs test was training programmes. This is helpful not only during
applied to ANMI or AFAL results. checking and calibration procedure, but also in the over-
Significant differences between the results given by all analytical procedure, since a large number of vita-
the two analysts ANMI and AFAL were detected for both mins analysis measurements are based on volumetric
types of volumetric glassware. jEn-scorej > 1 was ob- measurements (Klejdus et al., 2004; Sharpless, Margolis,
served for flasks and pipettes indicating that the results & Thomas, 2000).

Table 1
Overview of statistical tests, applied to evaluate operatorÕs results
Flask En-score F-test Pipette En-score F-test
20 ml 50 ml 20 ml 50 ml 2 ml 5 ml 2 ml 5 ml
#1 22.5 26.4 9.00 4.00 #1 1.3 6.7 1.00 4.00
#2 14.8 15.6 1.00 1.00 #2 2.5 2.4 9.00 1.00
#3 3.1 7.4 4.00 1.00 #3 4.2 3.1 4.00 2.25
#4 22.6 10.7 1.00 4.00 #4 – 2.8 – 1.00
#5 4.5 9.9 4.00 1.00 #5 – 0.6 – 9.00
Criteria used to classify operatorÕs results: jEn-scorej > 1, unsatisfactory; jEn-scorej = 1, questionable; jEn-scorej < 1, satisfactory; F0.95(9,9) = 3.18.
724 I. Castanheira et al. / Food Control 17 (2006) 719–726

Deviation from the reference value due to tempera- glassware. Burfield and Hefter (1987) has concluded that
ture and exposure intervals is presented in Fig. 4. The for oven drying borosilicate glassware, the calibration
nominal capacity did not change when volumetric glass- value is not significantly affected. Our results are not
ware was maintained at 4 °C. These results are expected in agreement with BurfieldÕs conclusion possibly because
for borosilicate material (Burfield & Hefter, 1987). But the calibration methods and the uncertainty calculations
at 50 °C, significant effects were noticed, depending on applied here are different. In this study, uncertainty cal-
the type of volumetric glassware, capacity and exposure culations and the calibration process were determined
period. The highest deviation from reference value was through a metrological approach which is more rigorous
observed at day five for both types of volumetric glass- to investigate differences between or within measure-
ware and the largest effect was observed for pipettes of ments results (De Bièvre & Taylor, 1997).
1 ml (Fig. 5). The results in the present study show that In daily use, machine washing and oven or air drying
temperature effect is different according to temperature of glassware at moderate temperatures (around 60 °C)
value, period of time, type and capacity of volumetric are unavoidable, for volumetric glassware used with
complex food matrices. Therefore, the glassware should
be submitted to a qualification performance test regu-
0.006 larly (Bedson & Sargent, 1996; UKAS, 2002).
4 ºC Fig. 6 shows the mean bias due to volumetric glass-
ware in the determination of vitamins content. Persistent
Deviation from reference value (%)

50 ºC
0.002 bias (Taverniers, De Loose, & Bockstaele, 2004), is de-
fined as the difference between the expectation of the test
results (protocol B) and the reference value (protocol
-0.002
A). Potential bias due to volumetric glassware was
investigated in all steps of the analytical procedure for
the determination of vitamins content and the largest
-0.006
contribution to bias was observed for the calibration
curve and extraction step.
-0.010 The operatorÕs performance and temperature effects
on volumetric glassware are the factors that influence
the most the nominal capacity. This enabled us to
-0.014 demonstrate that lack of accuracy can overestimate the
1 3 5 value of vitamins content, in the range of 1–11%, except
Time (days)
for Vitamin D where the results are unbiased. This
pattern of results strongly suggests the influence of
Fig. 4. Results of temperature tests for graduated pipettes as a
function of time.

0.4
Deviation from reference value (%)

0.3

0.2

0.1

0
1 2 5

Capacity of pipette (ml)

Fig. 6. Influence of bias due to volumetric glassware on reported value
Fig. 5. Temperature effect on nominal capacity of graduated pipettes of vitamin concentration. The largest source comes from low capacity
after five days at 50 °C. glassware.
 I. Castanheira et al. / Food Control 17 (2006) 719–726
systematic errors in the preparation of the calibration
curve. Vitamin D was quantified using an internal stan-
dard and for the other vitamins, the content was calcu-
lated by regression analysis using a calibration curve
with five external standards, which were prepared by a
dilution procedure. The largest bias was observed for
vitamin B1, perhaps due to the high amount of volumet-
ric glassware used in the analytical procedure, especially
during the preparation of calibration curve. For vita-
mins A, E and B2, bias is introduced by low capacity
volumetric glassware (pipettes and flasks) and for vita-
min B6 bias is due to pipettes of 2 ml and 5 ml. The
results obtained when a small number of flasks and pip-
ettes are used did not differ significantly in both proto-
cols, while those obtained when a high number of low
capacity pipettes are used were systematically biased.
From this study, we conclude that a cumulative effect
of error in the dilution steps for the preparation of the
calibration curve is probably associated with the lack
of fit of linearity and can contribute significantly to less
accurate results. This study has implications concerning
routine work in the determination of vitamins content in
food and was motivated by the need of traceability and
comparability of results. Differences ranging from 10%
to 40% for the value of vitamin A, E, B1, B2 and B6
content have been reported by food analysis laborato-
ries and are largely connected with the expertise level
of participants (Part 1: Hollman et al., 1993a; Part 2:
Hollman et al., 1993b; Mathiasson et al., 2002). In the
determination of Vitamin A, in serum, the same conclu-
sion was reported (Hulshof, Brouwer, Burema, & West,
2002). Although variations in stability and integrity of
volumetric glassware can be relatively small when com-
pared to other sources of error, they need to be properly
evaluated as defined by item no. 5.9.1, in the new
revision of ISO 17025 (FDIS ISO 17025, 2004), and
are necessary to improve collaborative tests results and
inter-laboratory comparability. This work raises the
problem of correlating the nominal capacity variation
which occurs in daily used volumetric glassware with
the overestimation content of vitamins. Therefore, our
results can contribute to improve the evaluation of
laboratory performances and comparability of results
as recommended by Codex Alimentarius (Codex, 2002).
4. Conclusions
The present methodology evaluates the factors affect-
ing the accuracy of volumetric glassware. This approach
is robust and feasible, thus, enabling its adoption in
food analysis laboratories.
This study highlights the critical control points of lab-
oratory volumetric glassware addressing the need of
periodic check intervals and calibration in the measure-
ment plan.
725
Furthermore, collaboration between food analysis
and metrological laboratories, reveals to be very useful:
(a) to provide support for education and training of per-
sonnel; (b) to improve the traceability of working level
by increasing the quality of link to SI units of assigned
values and associated uncertainties; (c) to support the
organization of inter-laboratory comparisons, a tool to
assess the ability of food laboratories to generate data
quality that may be utilized in aims such as establish-
ment of food/disease-health-status using different
sources of analytical data.
Acknowledgments
The authors would like to thank Dr. Maria Antónia
Calhau, Head of Department-INSA and to Engo Antó-
nio Cruz, Director of IPQ/LCM for encouragement of
this work, to Dr. Luı́sa Oliveira and Enga Eduarda Fil-
ipe, MD for providing laboratory facilities and to Hel-
ena Bártolo for vitamins analysis. This work was
partially supported by PIDDAC/IPQ/LCM/Universid-
ades (1997–2004) and POCTI /CTA/95/2001.
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