ISSN 1831-9424

Determination of melamine and

formaldehyde (FA) in food contact
material migration solutions.
FCM-23/01 Proficiency Test Report

Bratinova, S.P., Robouch, P., Beldi, G., Senaldi, C.,

Hoekstra, E.
268-PT

2024

EUR 31926 EN
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JRC137627

EUR 31926 EN

PDF ISBN 978-92-68-15427-4 ISSN 1831-9424 doi:10.2760/42351 KJ-NA-31-926-EN-N

Luxembourg: Publications Office of the European Union, 2024

© European Union, 2024

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How to cite this report: European Commission, Joint Research Centre, Bratinova, S.P., Robouch, P., Beldi, G., Senaldi, C. and Hoekstra, E.,
Determination of melamine and formaldehyde (FA) in food contact material migration solutions., Publications Office of the European Union,
Luxembourg, 2024, https://data.europa.eu/doi/10.2760/42351, JRC137627.
Contents
Abstract …………………………………………………………………………………………………………………………..3
Acknowledgements ................................................................................................ 4
Executive summary ............................................................................................... 5
1 Introduction ......................................................................................... 6
2 Scope ................................................................................................. 6
3 Set up of the exercise ........................................................................... 6
3.1 Quality assurance....................................................................................... 6
3.2 Confidentiality ........................................................................................... 6
3.3 Time frame ............................................................................................... 7
3.4 Distribution ............................................................................................... 7
3.5 Instructions to participants .......................................................................... 7
4 Test items ........................................................................................... 8
4.1 Preparation ............................................................................................... 8
4.2 Homogeneity and stability ........................................................................... 8
5 Assigned values and corresponding uncertainties ...................................... 9
5.1 Assigned values ......................................................................................... 9
5.2 Associated uncertainties.............................................................................. 9
5.3 Metrological traceability of the assigned value ............................................... 9
5.4 Standard deviation for proficiency assessment, σpt ......................................... 9
5.5 Compliance statement for test item 2 ......................................................... 10
6 Evaluation of results ........................................................................... 10
6.1 Scores and evaluation criteria .................................................................... 10
6.2 General observations ................................................................................ 12
6.3 Laboratory results and scorings ................................................................. 12
6.3.1. Performances ............................................................................ 12
6.3.2. Truncated values ....................................................................... 13
6.3.3. Measurement uncertainties ......................................................... 13
6.3.4. Test item 2 compliance statement evaluation ................................ 13
6.3.5. Observations on the compliance assessment of test item 2 ............. 19
6.3.6. Additional information extracted from the questionnaire ................. 20
7 Conclusion ......................................................................................... 21
References 23
List of abbreviations and symbols .......................................................................... 24
List of figures...................................................................................................... 25
List of tables ....................................................................................................... 25

1
 A. Announcement of the PT round “FCM-23/01” ..................................... 26
Annex 1: B. Invitation letter .............................................................................. 27
Instructions for participants ................................................................. 28
Questionnaire .................................................................................... 31
Homogeneity and stability results ......................................................... 34
A. Homogeneity study for test item 1, all values in mg kg-1 .............................. 34
B. Homogeneity study for test item 2, all values in mg kg-1 ............................... 34
C. Stability study at 40oC, 20oC and 4oC (RT) for one and/or 13 weeks all values in
mg kg-1 (REF, reference) ............................................................................ 35
Results for melamine in FS.B (test item 1) ............................................. 36
Results for formaldehyde in FS.B (test item 1) ....................................... 38
Repeated temperature profiles (3 consecutive migrations between 68 and
72 oC (Profile 1) performed by the EURL on a mug (test item 2) .............. 40
Three different temperature profiles within the recommended temperature
range of 70 ± 2 oC, obtained by the EURL for different mugs (test item 2) 41
Melamine results obtained by the EURL ................................................. 42
Formaldehyde migration results obtained by the EURL ............................ 43
Reported results for three consecutive migrations (m1, m2, m3) of melamine
in food simulant B from test item 2 (MUG), expressed in mg kg -1 ............. 44
Reported results for three consecutive migrations (m1, m2, m3) of
formaldehyde in food simulant B from test item 2 (MUG), expressed in mg
kg-1................................................................................................... 45
Results of the questionnaire ................................................................. 46

2
Abstract
The European Union Reference Laboratory for Food Contact Materials (EURL-FCM)
organised a proficiency testing round (FCM-23/01) for the determination of the mass
fraction of melamine and formaldehyde in food simulant B solutions, in support to
Commission Regulation (EU) 2020/1245. This proficiency testing exercise was open to
EU National Reference Laboratories (NRLs) and Official Control Laboratories (OCLs). The
EURL dispatched two well-characterised test items for analysis, namely (i) a food
simulant solution B spiked with the specified substances, and (ii) four bamboo/melamine
mugs for the migration tests. Twenty-five NRLs from 24 countries, and 18 OCLs (from
Belgium, Germany, Italy and Spain) reported results. Analysing the spiked solution
proved relatively straightforward, with over 95 % of the participants reporting
satisfactory results. However, the compliance assessment of the mugs was more
challenging; only 6 laboratories assessed correctly the compliance of test item 2 for both
melamine and formaldehyde in line with the observations of the EURL, while several
others presented compliance statements in line with the EURL but inconsistent with their
own experimental results. This report provides a detailed discussion about the outcomes
of this proficiency testing exercise.

3
Acknowledgements
The forty-three laboratories listed hereafter are kindly acknowledged for their
participation in the PT.
Organisation Country
AGES, Gebrauchsgegenstände Austria
Federal agency for the safety of the food chain (AFSCA-FAVV) Belgium
Sciensano Belgium
National Center of Public Health and Analyses (NCPHA) Bulgaria
Croatian Institute of Public Health (HZJZ) Croatia
State General Laboratory (SGL) Cyprus
National Institute of Public Health (SZÚ) Czech Republic
Technical University of Denmark (TUD) Denmark
Danish Veterinary and Food Administration (DVFA) Denmark
Finnish Customs (TULLI) Finland
Laboratoire National de Metrologie et d'essais (LNE) France
Service Commun des Laboratoires (SCL), Laboratoire de Bordeaux France
Chemisches und Veterinäruntersuchungsamt Münsterland-Emscher-Lippe (CVUA-MEL) Germany
Thüringer Landesamt für Verbraucherschutz (TLV) Germany
Landesbetrieb Hessisches Landeslabor (LHL), Hessen Germany
German Federal Institute for Risk Assessment (BfR) Germany
Chemisches- und Veterinäruntersuchungsamt (CVUA) Stuttgart (chemical & veterinary office) Germany
LAVES, Institut für Bedarfsgegenstände Lüneburg (IfB) Lüneburg Germany
Landeslabor Schleswig-Holstein (LSH) Germany
General Chemical State Laboratory (GCSL) Greece
National Food Chain Safety Office (NEBIH), Food Chain Safety Laboratory Directorate Hungary
The Public Analyst's Laboratory Ireland
Agenzia di Tutela della Salute (ATS)-Milano Italy
Istituto Zooprofilattico Sperimentale della Lombardia e dell'Emilia Romagna (IZSLER), Italy
Chemical Department Bologna
Agenzia Regionale per la Protezione Ambientale delle Marche (ARPAM), Laboratorio Chimico Italy
USL TOSCANA CENTRO, LABORATORIO DI SANITA PUBBLICA Italy
Agenzia regionale per la protezione dell'ambiente Friuli Venezia Giulia (ARPA FVG), Italy
Laboratorio di Udine
Agenzia di Tutela della Salute (ATS) Insubria, Laboratorio di Prevenzione Italy
Istituto Superiore di Sanità (ISS), Dipartimento Ambiente e salute (DAMSA) Italy
National Public Health Surveillance Laboratory (NPHSL) Lithuania
Laboratoire National de Santé (LNS) Luxembourg
Netherlands Food and Consumer Product Safety Authority (NVWA) Product Safety Laboratory Netherlands
Escola Superior de Biotecnologia - Universidade Católica Portuguesa Portugal
National Institute of Public Health (INSP) Romania
Regional Public Health Authority Slovakia
National Laboratory of Health, Environment and Food (NLZOH) Slovenia
Centro Analitico de Inspección y Control de Calidad de Comercio Exterior. SOIVRE Spain
Centro Nacional Alimentacion (CNA) Spain
Laboratorio de Salud Pública – Madrid Salud Spain
Laboratorio de Salud Pública de Alicante Spain
AINIA Centro Tecnologico Spain
Swedish Food Agency Sweden
Official Food Control Authority of the Canton of Zürich Switzerland

Authors
Stefanka Bratinova (PT coordinator),
Piotr Robouch, Giorgia Beldi, Chiara Senaldi, Eddo Hoekstra

This report has been authorised by Ursula Vincent, Head of Unit JRC F.5.

4
Executive summary
The European Union Reference Laboratory for Food contact materials (EURL-FCM)
organised a proficiency test (FCM-23/01) for the determination of melamine and
formaldehyde to support the Commission Regulation (EU) 2020/1245 amending
Regulation (EU) No 10/2011 on plastic materials and articles intended to come into
contact with food. This proficiency test was open to National Reference Laboratories
(NRLs) and Official Control Laboratories (OCLs).

Two test items were prepared and dispatched to participants for analysis. Test item 1
consisted of a solution of melamine and formaldehyde in food simulant B (acetic acid 3
% w/v in water), while test item 2 consisted of four bamboo/melamine mugs. The
homogeneity and stability of both test items were evaluated by the EURL while the
assigned values for test item 1 were derived from the gravimetrical preparation of the
solution. No assigned values were needed for test item 2.

Twenty-five NRLs from 24 countries and 18 OCLs registered to this PT round and
reported results. The results for test item 1 were rated using z and zeta (ζ) scores in
accordance with ISO 13528:2022. Relative standard deviations for proficiency
assessment (σpt) were set to 15 % of the respective assigned values for the two
analytes.

More than 95 % of the participating laboratories performed satisfactorily (according to

the z score) for the analysis of melamine and formaldehyde in the solution. These results
confirm the competence of the participants in effectively monitoring melamine and
formaldehyde in food simulant B.

The assessment of participants' compliance statements for test item 2 presented

significant difficulties. Minor variations in migration test conditions, though within the
tolerable range had a significant impact on the test results. Only 28 % (12 out of 43) of
the laboratories accurately assessed the compliance and the stability of migration for
formaldehyde in test item 2, in line with the EURL conclusion. The assessment of
melamine stability of migration and compliance with the specific migration limit (SML)
for test item 2 emerged as notably arduous with only 18 % (7 out of 39) of the laboratories
correctly assessing compliance and stability for melamine in test item 2, aligning with
the EURL conclusions.
In conclusion, assessing the compliance of melamine-bamboo mugs remains challenging
and requires further investigations.

5
1 Introduction
The European Union Reference Laboratory for Food Contact Materials (EURL-FCM),
hosted by the Joint Research Centre of the European Commission, organised a
proficiency test (PT) for the determination of melamine and formaldehyde in food
simulant B solution and their migration from melamine-bamboo ware to support the
Commission Regulation (EU) 2020/1245 [1].
This PT was agreed upon with the Directorate General for Health and Food Safety
(DG SANTE) as part of the EURL-FCM annual work programme 2023, thus complying
with the mandate set in Regulation (EU) 2017/625 [2]. The PT was open to National
Reference Laboratories (NRLs) and to Official Control Laboratories (OCLs) willing to
participate.

This report summarises the outcome of the PT.

2 Scope
The present PT aims to assess the performance of NRLs and OCLs in the determination
of melamine and formaldehyde in food simulant B and their migration from melamine-
bamboo ware. The PT was mandatory for the NRLs active in the field of FCM, and open
to OCLs. Participants were also asked to assess the compliance of the melamine-bamboo
mugs (test item 2) with the specifications outlined in Regulations (EU) 2020/1245 [1].
This PT, organised in line with ISO 17043:2023 [3], is identified as "FCM-23/01".

3 Set up of the exercise

3.1 Quality assurance

The JRC Unit hosting the EURL-FCM is accredited according to:

 ISO/IEC 17025:2017 [4] (certificate number BELAC 268-TEST)

 ISO/IEC 17043:2023 [3] (certificate number: BELAC 268-PT,

proficiency test provider)

The reported results were evaluated following the relevant administrative and logistic
procedures.

3.2 Confidentiality
The procedures used for the organisation of PTs guarantee that the identity of the
participants and the information provided by them is treated as confidential. The
participants in this PT received a unique laboratory code used throughout this report.
However, the laboratory codes of NRLs appointed in line with Regulation (EU) 2017/625
[3] may be disclosed to DG SANTE upon request for the purpose of an assessment of
their (long-term) performance. Similarly, laboratory codes of appointed OCLs may be
disclosed to their respective NRL upon request.

6
 3.3 Time frame
The organisation of the PT FCM-23/01 exercise was announced during the EURL-FCM
plenary meeting on October 12, 2022, and an additional email was sent in May 2023
(Annex 1a). An invitation letter was then sent to NRLs and OCLs on May 17, 2023
(Annex 1b). The registration deadline was set to June 12, 2023. Samples were sent to
participants on June 21, 2023. The deadline for reporting of results was first set to
August 25, 2023 (Annex 2), and later extended until September 6, 2023 upon request of
some participants.

3.4 Distribution
Each participant received:
 One vial containing 20 mL of food simulant B (acetic acid 3 % w/v) solution
spiked with melamine and formaldehyde (test item 1); and
 Four melamine-bamboo mugs (test item 2) for migration test of melamine and
formaldehyde in food simulant B.
Samples were sent under normal transport conditions at ambient temperature.

3.5 Instructions to participants

Detailed instructions were given to participants in the "Instruction letter” (Annex 2).
Participants were requested to inspect the vial and the mugs for damages upon arrival.
They were also instructed to store test item 1 in the refrigerator at 4 °C ± 2 °C in the
dark upon reception and until analysis, to minimise the risk of contamination and ensure
stability. Analyses were to be conducted soon after reception.
For test item 1, participants were requested to determine the “mass fraction of
melamine and formaldehyde in the food simulant B solution” and subsequently
report the results and the corresponding expanded measurement uncertainties in
mg kg-1. This calculation was to be performed assuming a density of 1 kg m -3 for the
food simulant B solution. Results were to be reported using the same number of
significant figures normally reported to customers.

Similarly, participants were requested:

- to treat test item 2 as routine samples;
- to perform three consecutive migration experiments (m1, m2 and m3) at 70 ± 2 °C
for 120 ± 5 minutes, on three different mugs (MUG1, MUG2 and MUG3), following
their routine procedures;
- to determine the “mass fraction of melamine and formaldehyde” migrated from the
mugs into the food simulant B solution, and to assess the compliance of the mugs
with the specifications outlined in Commission Regulation (EU) 2020/1245 [1].

Participants received an individual code to access the on-line reporting interface, to

report their measurement results and to complete the related questionnaire. The latter
was designed to gather additional information related to measurements and laboratories
(Annex 3).

Random laboratory codes were attributed and individually communicated to participants

by e-mail.

7
4 Test items

4.1 Preparation
Test item 1 consisted of a food simulant B solution spiked with melamine and
formaldehyde.

Formaldehyde stock solution (LRAD2648 CRM 998 mg/L) was purchased from Sigma
Aldrich, while the melamine stock solution was prepared by weighing ca. 50 mg of pure
standard (Sigma Aldrich MKCP8204) in 100 mL volumetric flasks and filled to the mark
with water. The bulk solution of test item 1 was prepared by transferring ca. 25 mL of
formaldehyde and 10 mL of melamine stock solutions into a 2 L volumetric flask,
subsequently filled to the mark with food simulant B solution. Individual test items were
prepared by transferring 20 mL of the bulk solution into 22 mL glass vials, resulting in a
total of 100 vials produced. Each vial was uniquely identified with a number and the PT
identifier. The mass fractions of formaldehyde and melamine in both solutions were
determined as described in Section 5.1.

A total of 250 melamine/bamboo mugs were purchased from a local market. Each
participant received a set of four mugs (test item 2) to conduct the migration tests.

4.2 Homogeneity and stability

Measurements for the homogeneity and stability studies and the statistical treatment of
data were performed by the EURL-FCM.
The melamine in food simulant B (acetic acid 3 % w/v) solution was determined by high
performance liquid chromatography (HPLC) using UV detection at 220 nm. The
formaldehyde analysis involved mixing food simulant B with 2,4-dinitrophenylhydrazine
(DNPH) to form the corresponding hydrazine, followed by HPLC-UV detection at 360 nm.

Homogeneity assessment was performed after the preparation of the test items and
before distribution to participants.

For test item 1, ten vials were randomly selected and analysed in duplicate. Results
were evaluated according to ISO 13528:2022 [5]. The solution proved to be
adequately homogeneous for the investigated analytes (Annex 4.A). The
contribution from homogeneity (uhom) to the standard uncertainty of the assigned
value (u(xpt)) was calculated using SoftCRM [6].

The homogeneity test played a critical role for test item 2, due to the difficulty in
finding a large batch of commercial mugs that was sufficiently homogeneous. The
homogeneity study was conducted for three consecutive migrations (m1, m2 and
m3) at 70 ± 2 oC for 120 ± 5 min, using 10 randomly selected mugs, and focusing
on both melamine and formaldehyde. Due to the “destructive” nature of the test,
no replicate analyses were feasible. Sufficient homogeneity was proven based on
the reasonable relative standard deviations (below 10 %) observed in the
migrations and the analyses of the selected mugs (Annex 4.B).

Stability assessment was conducted at two points: (i) immediately after the preparation
of the test items (time 0) and (ii) after the reporting of results.

Three additional samples of the solution (test item 1) were analysed in duplicate
after the reporting deadline. Results were then compared to those obtained from

8
 the homogeneity study. This stability study confirmed that test item 1 was
adequately stable (i) at room temperature (20oC) over the entire PT period (13
weeks, from the value assignment until the deadline for reporting results); (ii) for
1 week at 40 °C (simulating extreme conditions which may occur during
transport); and (iii) at the reference temperature of 4 °C. Hence, the uncertainty
contribution due to stability was set to zero (ust = 0) for all the investigated
analytes (Annex 4.C).
No stability study was conducted for test item 2, as the mugs were assumed to be
stable with the time and thus also the migration of melamine and formaldehyde
from them.

5 Assigned values and corresponding uncertainties

5.1 Assigned values

The assigned values (xpt) for melamine and formaldehyde in test item 1 were derived
from formulation (Table 1).

5.2 Associated uncertainties

The associated standard uncertainties of the assigned values (u(xpt)) for melamine and
formaldehyde in test item 1 were calculated following the law of uncertainty propagation,
combining the standard measurement uncertainty of the characterisation (uchar) with the
standard uncertainty contributions from homogeneity (uhom) and stability (ust), in
compliance with ISO 13528:2022 [5]:

𝑢(𝑥𝑝𝑡 ) = √𝑢2𝑐ℎ𝑎𝑟 + 𝑢2ℎ𝑜𝑚 + 𝑢2𝑠𝑡 Eq. 1

The uncertainty uchar was estimated from the formulation following the law of uncertainty
propagation, combining quadratically the standard deviations of the input quantities as
recommended by the Guide of expression of uncertainty in measurement (GUM) [7].

5.3 Metrological traceability of the assigned value

The assigned values were obtained by gravimetric preparation from Sigma-Aldrich’s
standards. The SI-traceable calibration of balances and a thorough control of the
weighing procedure ensure traceability of the weighing itself.

5.4 Standard deviation for proficiency assessment, σpt

The relative standard deviations for proficiency assessment (σpt,rel) of melamine and
formaldehyde in test item 1 were set to 15 % of the respective assigned values, based
on expert judgment (Table 1).
Table 1: Assigned values (xpt) and standard deviation for the PT assessment (σpt)
for melamine and formaldehyde in test item 1 (T1).
All values (excluding last column) are expressed in mg kg-1.

Measurand xpt uchar uhom u(xpt) k = 1 σpt (σpt,rel) u(xpt)/σpt

Melamine in T1 2.528 0.0058 0.0037 0.0069 0.379 (15 %) 0.02

Formaldehyde in T1 12.48 0.21 0.01 0.21 1.87 (15 %) 0.11

9
 5.5 Compliance statement for test item 2
Commission Regulation (EU) 2020/1245 introduced the requirement for a plastic
repeated-use article to be stable during three consecutive migrations. According to the
note on “Options for checking compliance of plastic food contact material articles for
repeated use - An EURL-FCM harmonised approach (Ares(2022)8554518)” sent by the
EURL to DG SANTE, the sample shall be considered non-compliant for the migration of a
substance considering the standard measurement uncertainty if:
𝑚3 > 𝑆𝑀𝐿, or
𝑚2 > 𝑚1 𝑂𝑅 𝑚3 > 𝑚2

These criteria shall be evaluated as follows:

Crit.1: IF (𝒎𝟑 − 𝑺𝑴𝑳 )/[(𝒖(𝒎𝟑)] > 𝟏. 𝟔𝟒 THEN 𝒎𝟑 > 𝑺𝑴𝑳

Crit.2: IF (𝒎𝒋 − 𝒎𝒊 )/[(𝒖(𝒎𝒋) + 𝒖(𝒎𝒊)] > 𝟏. 𝟔𝟒 THEN 𝒎𝒋 > 𝒎𝒊

For a harmonised approach the standard measurement uncertainty (u) is calculated by

the modified Horwitz method.

The plastic mugs investigated are designed for repeated-use with hot-fill applications. As
per Regulation (EU) No 10/2011 [10], the migration of substances from the mugs should
be tested at 70 °C for 2 hours. Furthermore, the normative Annex C of the EN 13130-
1:2004 standard [11] defines tolerance ranges for both contact temperature and time, of
70 ± 2 °C and 120 ± 5 min, respectively.

In a series of three consecutive migrations (m1, m2 and m3) from the same mug,
performed by the EURL-FCM, a repeatable temperature profile (profile 1) was observed
in the food simulant B (Annex 7), falling within the specified tolerance limits. This
consistency ensures the accuracy of the migration results.
Compliance with the SML and the stability of test item 2 were assessed based on the
homogeneity results (Annex 4B). The third migration of formaldehyde into food
simulant B was significantly below the SML of 15 mg kg-1, and the consistency observed
across the three migrated levels confirmed the stability of the mugs (Annex 10A).
Consequently, test item 2 is considered to be compliant for formaldehyde. On the
contrary, the third migration of melamine into food simulant B exceeded significantly the
SML of 2.5 mg kg-1. Despite exhibiting stable behaviour throughout the three migrations
(Annex 9A), the test item 2 is considered non-compliant for melamine.

6 Evaluation of results

6.1 Scores and evaluation criteria

The individual laboratory performance was expressed in terms of z and ζ scores
according to ISO 13528:2022 [5]:

xi  x pt
z Eq. 2
σ pt

10
 xi  x pt
  Eq. 3
u ( xi )  u 2 ( x pt )
2

Where: xi is the measurement result reported by a participant;

u(xi) is the standard measurement uncertainty reported by a participant;

xpt is the assigned value;

u(xpt) is the standard measurement uncertainty of the assigned value;

pt is the standard deviation for proficiency test assessment.

The interpretation of the z and ζ scores is done according ISO 13528:2022 [5]:
|score| ≤ 2 satisfactory performance (green in Annexes 5-6)
2 < |score| < 3 questionable performance (yellow in Annexes 5-6)
|score| ≥ 3 unsatisfactory performance (red in Annexes 5-6)

The z scores compare the participant's deviation from the assigned value with the
standard deviation for proficiency test assessment (pt) used as common quality criterion.

The ζ scores state whether the laboratory's result agrees with the assigned value within
the respective uncertainty. The denominator is the combined uncertainty of the assigned
value u(xpt) and the measurement uncertainty as stated by the laboratory u(xi). The ζ score
includes all parts of a measurement result, namely the expected value (assigned value),
its measurement uncertainty in the unit of the result as well as the uncertainty of the
reported values. An unsatisfactory ζ score can either be caused by an inappropriate
estimation of the concentration, or of its measurement uncertainty, or both.
The standard measurement uncertainty of the laboratory u(xi) was obtained by dividing
the reported expanded measurement uncertainty by the reported coverage factor, k.
When no uncertainty was reported, it was set to zero (u(xi) = 0) by the PT coordinator.
When k was not specified, the reported expanded measurement uncertainty was
considered by the PT coordinator as the half-width of a rectangular distribution; u(xi) was
then calculated by dividing this half-width by √3, as recommended by Eurachem [8].

Uncertainty estimation is not trivial, therefore an additional assessment was provided to

each laboratory reporting measurement uncertainty, indicating how reasonable their
measurement uncertainty estimation has been. The relative standard measurement
uncertainty was calculated based on the absolute values of the assigned values
[urel(xpt) =100*(u(xpt)/xpt)] and of the reported values [urel(xi)=100*(u(xi)/xi)].
The relative standard measurement uncertainty from the laboratory urel(xi) is most likely
to fall in a range between a minimum and a maximum allowed uncertainty (case "a":
umin,rel ≤ urel(xi) ≤ umax,rel). umin,rel is set to the standard uncertainties of the assigned
values urel(xpt). It is unlikely that a laboratory carrying out the analysis on a routine basis
would determine the measurand with a smaller measurement uncertainty than the
expert laboratories chosen to establish the assigned value (ISO 13528:2022 §7.6) or, if
applicable, by formulation (ISO 13528:2022 §7.3) or than the certified measurement
uncertainty associated with a certified reference material property value (ISO
13528:2022 §7.4). umax,rel is set to the standard deviation accepted for the PT
assessment, σpt (expressed as a percentage of the assigned value). Consequently, case
"a" becomes: urel(xpt) ≤ urel(xi) ≤ σpt,% .

11
If urel(xi) is smaller than urel(xpt) (case "b") the laboratory may have underestimated its
measurement uncertainty. Such a statement has to be taken with care as each
laboratory reported only measurement uncertainty, whereas the measurement
uncertainty associated with the assigned value also includes contributions for
homogeneity and stability of the test item. If those are large, relative measurement
uncertainties smaller than urel(xpt) are possible and plausible.
If urel(xi) is larger than σpt,% (case "c") the laboratory may have overestimated its
measurement uncertainty. An evaluation of this statement can be made when looking at
the difference between the reported value and the assigned value: if the difference is
smaller than the expanded uncertainty U(xpt) then overestimation is likely. If the
difference is larger but xi agrees with xpt within their respective expanded measurement
uncertainties, then the measurement uncertainty is properly assessed resulting in a
satisfactory performance expressed as a ζ score, though the corresponding performance,
expressed as a z score, may be questionable or unsatisfactory.

It should be pointed out that "umax,rel" is a normative criterion when set by legislation.

6.2 General observations

Twenty-five NRLs from 24 Member States and Switzerland, and twenty OCLs (from
Germany, Italy, Spain and Belgium) registered to the exercise. Two OCLs did not report
results. The remaining 43 laboratories, represent most of the EU Member States (except
Poland, Estonia and Malta). In addition, three NRLs and 2 OCLs reported results only for
formaldehyde.

6.3 Laboratory results and scorings

6.3.1. Performances
The laboratory performance for melamine and formaldehyde in test item 1 was
evaluated using z and  (zeta) scores

Annexes 5 and 6 present the reported results as tables and graphs for both measurands.
NRLs and OCLs are denoted as LNxx and LOxx, respectively.

Figure 1 summarises the performance scores obtained, with a total of 38 and 43 results
scored for melamine and formaldehyde, respectively. Overall, a very good performance
("satisfactory” according to the z score) is observed for 95 % and 98 % of the results
reported for melamine and formaldehyde, respectively. Similarly, the evaluation of the
laboratory performance, according to the zeta scores, was satisfactory for over 70 % of
the reported results. Two unsatisfactory (blunder) results were reported, one for
melamine and one for formaldehyde, likely attributable to incorrect dilution factors used:
a factor of 100 for LN19 for melamine, and a factor of 10 for LN15 for formaldehyde.
The robust statistics, calculated using the Excel add-in developed by the Statistical
Subcommittee of the Analytical Methods Committee of the UK Royal Society of
Chemistry [9], yielded the following results: 2.47 ± 0.13 (5 %) mg kg -1 for melamine
and 12.2 ± 0.7 (6 %) mg kg-1 for formaldehyde. These values are in good agreement
with the assigned values by the EURL and presented in Table 1. The low robust standard
deviations observed suggest that the value of σpt (set to 15 % in this PT) could be
decreased for future PT assessments.

12
 Melamine
Figure 1:
MU 27 3 8
Overview of laboratory
performance per measurand
zeta 28 3 7 according to z and ζ scores for
formaldehyde and melamine in
z score
test item 1. Corresponding
36 11
number of laboratories are
test item1

included in the graph.

0% 20% 40% 60% 80% 100%

Formaldehyde Satisfactory, questionable and

unsatisfactory performances (z
MU 32 4 7 and zeta scores) are indicated in
green, yellow and red,
respectively.
zeta 36 2 5
Realistic, underestimated and
overestimated measurement
z score 42 01
uncertainties (a,b,c) are indicated
in blue, white and grey,
0% 20% 40% 60% 80% 100%
respectively.

6.3.2. Truncated values

Laboratory LN15 reported an unrealistic truncated value (< 1.86 mg kg-1) for melamine
in test item 1, while the assigned value for this measurand is 2.528 mg kg-1 (Table 1).

6.3.3. Measurement uncertainties

The majority of laboratories reporting quantitative results provided expanded
measurement uncertainties (MU) and coverage factors. However, two NRLs and two
OCLs did not report MU for melamine, and one NRL and one OCL did not provide them
for formaldehyde. Additionally, three participants did not report the coverage factor
applied. Nevertheless, Figure 1 shows that over 70 % of the participants provided
realistic evaluation of the measurement uncertainty.

6.3.4. Test item 2 compliance statement evaluation

Participants were requested to perform three consecutive migration experiments (m1,
m2 and m3) at 70 ± 2 °C for 120 ± 5 minutes, on three different mugs (MUG1, MUG2
and MUG3 – test item 2), following their routine procedures. They were then requested
to determine the “mass fraction of melamine and formaldehyde” migrated from the
mugs into the food simulant B solution, and to assess the compliance of the mugs with
the specifications outlined in Commission Regulation (EU) 2020/1245 [1]. In addition,
participants were requested to provide (i) information about their migration procedures
in the questionnaire, and (ii) the temperature profile measured in the food simulant.

The final compliance statements should align with the participants' data and conform to
the requirements outlined in Commission Regulation (EU) 2020/1245, specifically
Section 2.1.6 of Annex V, which prescribes compliance rules for "Repeated use materials
and articles." According to these requirements, evaluating the compliance of a repeated-
use article involves two key assessments: (i) verifying compliance with the Specific
Migration Limits (SML), and (ii) assessing the stability of the article by comparing results
from two consecutive migrations ((m1,m2) and (m2,m3)).

13
 Most of the laboratories submitted the following information for melamine and
formaldehyde in three different mugs (MUG1, MUG2, MUG3):
- Results from three migration tests (m1, m2, m3);
- Associated expanded uncertainty for the 1st migration test, U(m1)*;
- Corresponding coverage factor used, k
- Compliance statement for test item 2; and
- Temperature profile used for the migration tests.
(*) Note: Although laboratories provided the expanded uncertainty for the first
migration only, the EURL calculated the standard measurement uncertainty by dividing
the expanded uncertainty by the coverage factor (u(m1) = U(m1)/k), and the
corresponding relative standard deviation was calculated by dividing the standard
measurement uncertainty by the migration value (RSD = u(m1)/m1), which was
assumed to be constant for similar migration levels (RSD(m1) = RSD(m2) = RSD(m3).

The analytical results reported by the participants for three consecutive migration tests
(m1, m2, m3) of melamine and formaldehyde from test items 2 are presented in
Annexes 11 and 12. A summary overview is presented in Figure 2, grouped by mugs.

MUG1 MUG2 MUG3

Melamine
Formaldehyde

Figure 2: Box plots of the melamine and formaldehyde results reported by the
participants for the three consecutive migrations (m1, blue; m2, orange; m3,
grey) from three mugs (MUG 1-3), (migration in mg kg-1)

14
The EURL performed the following evaluation of the participants’ data:
- Scrutinising all temperature profiles and categorised them as Satisfactory (S),
Questionable (Q) and Unsatisfactory (U), as indicated in Table 2 and the last
column of Annexes 11-12;
- Comparing each third migration result with the relevant SML (Example 1) and
flagging values higher than SML with a pink cell in Annexes 11-12; and
- Examining consecutive migrations (m2, m1) and (m3,m2) (Example 2) to identify
increases in migrated levels, and flagging any such increase with the symbol “”.

These calculations were performed for all the reported results.

Example 1: Is a migrated level (m3) above SML? Crit.1

Melamine (Annex 11)
SML = 2.5 mg kg-1
LN01, MUG3

m1 = 2.59 mg kg-1
U(m1) = 0.259 mg kg-1; k = 1.73
u(m1) = 0.259 / 1.73 = 0.15 mg kg-1
RSu(m1)=RSu(m3)= 0.15 / 2.59 = 5.8 %

m3 = 2.9 mg kg-1
u(m3) = 0.058 * 2.9 = 0.17
Crit.1: (2.9 – 2.5) / 0.17 = 2.39 > 1.64
 m3 > SML

Example 2: Are the migrated levels stable?

Melamine (Annex 11) Formaldehyde (Annex 12)
LN08, MUG2 LN14, MUG3
m1 = 9.3 mg kg-1;
m1 = 1.4 mg kg-1;
U(m1) = 0.34 mg kg-1; k = 2 U(m1) = 2.12 mg kg-1; k = 2
u(m1) = 0.34 / 2 = 0.17 mg kg-1 u(m1) = 2.12 / 2 = 1.06 mg kg-1
RSu(m1)= 0.17 / 1.4 = 12.1 % RSu(m1)= 1.06 / 9.3 = 11.4 %
RSu(m1) = RSu(m2) = RSu(m3) RSu(m1) = RSu(m2) = RSu(m3)
m2 = 1.46 mg kg-1 m2 = 10.95 mg kg-1
u(m2) = 1.46 * 0.121 = 0.18 mg kg-1 u(m2) = 10.95 * 0.114 = 1.25 mg
m3 = 2.45 mg kg-1 kg-1
u(m3) = 2.45 * 0.121 = 0.30 mg kg-1 m3 = 11.75 mg kg-1
u(m3) = 11.75 * 0.114 = 1.33 mg
Crit.2: (2.45 – 1.46) / (0.18 + 0.30) = kg-1
= 2.1 > 1.64
 m3 > m2 Crit.2: (11.75 – 10.95) / (1.25 +
1.46  2.45 1.33)
Depicted in Annex 11 as = 0.31 < 1.64
 m3  m2
Note: Four laboratories (LN02, LN26, LN27, LO48) seem to have reported expanded
uncertainty in %, rather than in mg kg-1. For further calculations, the EURL-FCM
considered these values as relative expanded uncertainties.

15
The EURL scrutinised the temperature profiles based on expert judgement. While
Regulation (EU) No 10/2011 [10] specifies the test conditions (time and temperature)
for plastic food contact material and articles, it does not provide tolerance intervals. The
only document referring to tolerance ranges for time and temperature during the
migration experiment is the normative Annex C of EN 13130-1:2004 [11], which
establishes the following tolerance ranges for migration tests: 120 ± 5 min and
70 ± 2 oC, for contact time and temperature, respectively. These values were used for
evaluation of the temperature profiles together with expert judgement. The result of this
evaluation is reported in Table 2 using three quality categories: Satisfactory,
Questionable and Unsatisfactory.
Annexes 11 and 12 present the evaluation conducted by the EURL based on the two
criteria for the 9 results reported by the 43 laboratories for the three migrations in three
mugs. The following assessment process was applied:

Criterion 1 (m3 ≤ SML) is considered fulfilled (yes) for each laboratory when the
three results (M1m3, M2m3 and M3m3) are proven not to exceed the Specific
Migration Limit (SML) taking the standard measurement uncertainty in
consideration. When the value of m3 is at or below SML, assessing Criterion 1 is
straightforward, even in cases where measurement uncertainties are not
provided.

Criterion 2, addressing stability, is considered fulfilled (yes) when there is no

observed increase in migration for any consecutive migrations. This criterion
always requires knowledge of the laboratory's measurement uncertainty.

Consequently, samples with stable migration results and with a third migration
result below the SML should be categorised as "Compliant." Similarly, non-stable
migration results or third migration results above the SML should be labelled as
"Non-Compliant." These logical conclusions should be compared with the
assessments provided by the laboratories to ensure coherence. A compliance
statement of a participant is regarded as coherent when supported by the data
provided.

However, this consistency was not always observed. Incoherent statements were
noted, such as laboratories declaring their samples (i) as "compliant" while
presenting experimental evidence of instability or values above the SML, or (ii) as
"non-compliant" when no extreme values or instability could be observed.

A detailed analysis of the reported results for test item 2 is presented hereafter.

16
 Melamine (see Table 2, 3 & Annex 11) Formaldehyde (see Table 2, 3 & Annex 12)
 Most of the laboratories (38 out of 44)  43 laboratories reported results (excl. LO47);
reported quantitative results; 5 laboratories  No truncated values were reported;
did not perform migration tests, while LN15
 The reported relative standard uncertainties
reported only truncated (“less than”)
(RSu) ranged from 2 to 26 %; while 6
values;
laboratories did not provide their MU.
 The reported relative standard uncertainties
 Except one outlier (LN22 - MUG1,m1), all the
(RSu) ranged from 3 to 27 %; while 6
381 reported values ranged from 1.2 to 16.5
laboratories did not provide their
mg kg-1, with a median value of 7.0 mg kg-1;
measurement uncertainties.
the third migration result never exceeded
 Except one outlier (LO47 - MUG2,m2), all the SML of 15 mg kg-1, when taking
the 340 reported values ranged from 0.3 measurement uncertainties into account,
and 5.8 mg kg-1, with a median value of 2.0, thus complying with Criterion 1 (m3-u ≤
hence bracketing the SML of 2.5 mg kg-1, as SML), as shown in the Kernel density plot [9]
shown in the Kernel density plot [9] below. below.

Kernel Density Plot Kernel Density Plot

Melamine Melamine
0.12
0.45

0.4 SML 0.1

0.35 SML
0.08
0.3

0.25
0.06
0.2

0.15 0.04

0.1
0.02
0.05

0 0
-2.5 0 2.5 5 7.5 -5 0 5 10 15 20 25 30
-0.05

 5 laboratories issued an “incoherent”  9 laboratories issued an “incoherent”

compliance statement that is contradicted compliance statement that is contradicted
by their experimental data. by their experimental data.
 7 laboratories gave a compliance statement
 5 laboratories gave a compliance statement
without reporting uncertainty, thus making
without reporting uncertainty, thus making
the evaluation impossible.
the evaluation impossible.
 All laboratories reported third migration
 9 laboratories reported some third
results equal to or below the SML.
migration results that exceeded the SML
whereas 28 other laboratories provided  Results from 21 laboratories demonstrated
values equal to or smaller than SML. This increasing levels in successive migrations,
confirms the challenge in determining the thus failing to comply with Criterion 2.
compliance for melamine, particularly when  15 laboratories presented experimental
values are close to the SML. evidence supporting the compliance and
 Results from 22 laboratories support the stability of formaldehyde in the mugs.
stability of the melamine migration from However, three of them (LN15, LO23, LO39)
the test item 2 whereas 10 laboratories erroneously assessed test item 2 as non-
observed the opposite. compliant. Therefore, only 12 of the
laboratories provided a compliance
 7 laboratories presented experimental
statement in line with the EURL conclusions.
evidence indicating the non-compliance of
melamine in the mugs due to stable
successive migrations but with the 3rd
migration above SML, aligning with the
EURL’s findings; one of them (LN11)
provided unsatisfactory temperature
profile.
Finally, only 6 laboratories assessed correctly the compliance of test item 2 for both
melamine and formaldehyde in line with the observations of the EURL.

17
Table 2: Comprehensive presentation detailing compliance statements of the
participants (“statement”) related to melamine (M) and formaldehyde (F),
stability (“stable”) and compliance with SML (“<SML”) assessed by EURL,
coherence of their statement to their data (“coherence”), the calculated
relative standard uncertainty (“RSu (k=1)”), the evaluation of the temperature
profile used for migration (“T-profile”; S, satisfactory; Q, questionable; U,
unsatisfactory) and the overall agreement with the EURL conclusions
(“OVERALL”).

Melamine Formaldehyde
Lab Statement Stable < SML coherence RSu (k=1) Lab Statement Stable < SML coherence RSu (k=1) T profile OVERALL
LN01 NC yes no yes 6% LN01 C yes yes yes 12% S MF
LN02 C yes yes yes 11% LN02 NC no yes yes 4% Q
LN03 C yes yes yes 8% LN03 C no yes no 6% U
LN04 not tested LN04 NC no yes yes 8% U
LN05 NC ? ? ? LN05 NC ? yes ? S
LN06 not tested LN06 NC ? yes ? S
LN07 NC no yes yes 6% LN07 NC no yes yes 6% S
LN08 NC no yes yes 12% LN08 NC no yes yes 6% Q
LN09 C no yes no 3% LN09 C no yes no 6% U
LN10 C yes yes yes 13% LN10 C yes yes yes 10% U F
LN11 NC yes no yes 10% LN11 NC no yes yes 8% U M
LN12 C ? yes ? LN12 C ? yes ? Q
LN13 NC yes no yes 15% LN13 C yes yes yes 14% S MF
LN14 NC yes no yes 14% LN14 C yes yes yes 12% Q MF
LN15 NC yes yes no LN15 NC yes yes no 10% S F
LN16 C yes yes yes 7% LN16 C yes yes yes 5% F
LN17 NC no yes yes 3% LN17 NC no yes yes 7% Q
LN18 NC yes no yes 4% LN18 C yes yes yes 10% S MF
LN19 C yes yes yes 10% LN19 C no yes no 10%
LN20 C yes yes yes 20% LN20 C yes yes yes 15% S F
LN21 NC yes no yes 13% LN21 C yes yes yes 12% U MF
LN22 not tested LN22 ? no yes ? 2% U
LN23 NC no yes yes 7% LN23 NC yes yes no 19% S F
LN24 C yes yes yes 17% LN24 NC no yes yes 12% S
LN25 NC yes no yes 5% LN25 C yes yes yes 3% S MF
LN26 NC no yes yes 6% LN26 NC no yes yes 2% S
LN27 C yes yes yes 15% LN27 C no yes no 5% S
LO30 NC no no yes 6% LO30 NC no yes yes 7% S
LO31 C yes yes yes 27% LO31 C yes yes yes 26% S F
LO32 NC ? ? ? LO32 C ? yes ? S
LO33 C ? yes ? LO33 NC ? yes ? S
LO34 C yes yes yes 14% LO34 C yes yes yes 7% S F
LO35 C ? yes ? LO35 C no yes no 5% Q
LO36 C yes yes yes 21% LO36 C yes yes yes 16% U F
LO37 NC yes yes no 15% LO37 NC ? yes ? 17% Q
LO38 C yes yes yes 17% LO38 NC ? yes ? Q
LO39 NC yes yes no 25% LO39 NC yes yes no 13% S F
LO40 not tested LO40 NC no yes yes 18% Q
LO43 NC no yes yes 14% LO43 NC no yes yes 11% S
LO44 NC yes yes no 17% LO44 NC no yes yes 10% Q
LO45 C yes yes yes 5% LO45 NC no yes yes 5% S
LO46 not tested LO46 C no yes no 11% S
LO47 NC no no yes 5% LO47 not tested
LO48 NC no yes yes 10% LO48 NC no yes yes 5% S

18
Table 3 Summarised overview of the compliance statements of the laboratories for
melamine (non-compliant) and formaldehyde (compliant), reported stability,
reported compliance with SML, corresponding number of laboratories,
coherence of their statement, agreement with the EURL conclusions.

Melamine, assumed “Non-Compliant

coherent with
Lab.statement Stable? < SML? Nr experiment? aligned with EURL Labs
NC yes no 7 yes Yes LN01; LN11; LN13; LN14; LN18; LN21; LN25
NC yes yes 4 no LN15; LO37; LO39; LO44
NC no no 2 yes LO30; LO47
NC no yes 7 yes LN07; LN08; LN17; LN23; LN26; LO43; LO48
NC ? ? 2 LN05; LO32
C yes yes 13 yes LN02; 03; 10; 16; 19; 20; 24; 27; LO31; 34; 36; 38; 45
C no yes 1 no LN09
C ? yes 3 LN12; LO33; LO35
not tested -- -- 5 LN04; LN06; LN22; LO40; LO46
(?): no MU total 44

Formaldehyde, assumed “Compliant”

coherent with
Lab.statement Stable? < SML? Nr experiment? aligned with EURL Labs
C yes yes 12 yes Yes LN01; 10; 13; 14; 16; 18;20; 21; 25; LO31; 34; 36
C no yes 6 no LN03; LN09; LN19; LN27; LO35; LO46
C ? yes 2 LN12; LO32
NC yes yes 3 no LN15; LN23; LO39
NC no yes 14 yes LN02; 04; 07; 08; 11; 17; 24; 26; LO30; 40; 43; 44; 45; 48
NC ? yes 5 LN05; LN06; LO33; LO37
-- no yes 1 LN22
not tested -- -- 1 LO47
(?): no MU total 44

6.3.5. Observations on the compliance assessment of test item 2

Given the significant variations observed in compliance statements across laboratories,
the novelty of compliance assessment for NRLs and OCls, and the large variety of
temperature profiles reported by the laboratories, in addition to migrated levels of
melamine in food simulant B close to the SML, the EURL-FCM conducted an additional
experiment. This experiment aimed to assess the impact of temperature tolerance in the
food simulant on the compliance of test item 2. Initially, a migration test was conducted
on three different mugs, using slightly different oven settings while ensuring that the
temperature profiles remained within the tolerance range of 68 – 72 oC (see Annex 8).

Annex 7 demonstrates the EURL’s ability to replicate the temperature profile for
consecutive migrations for test item 2. This is important for obtaining repeatable
migration results (Annexes 9A and 10A).

Annex 8 shows that different temperature profiles can occur in the food simulant during
migration, with ranges 68 - 72 oC, 67.8 - 69.5 oC, and 67.3 - 68.3 oC, the latter
exceeding the tolerance range for 15 minutes. Annexes 9B and 10B show that the
migration levels increase with higher “average” temperature of the food simulant.
Specifically for melamine (Annex 9B), migrations with (lower) temperature profiles
outside the tolerance range exhibit significantly lower levels compared to those within
the tolerance range. A similar trend is observed for formaldehyde (Annex 10B).

19
In the case of melamine, migration levels significantly below the SML indicate
compliance when the temperature profile is lower, whereas the migration is significantly
above the SML, indicating non-compliance, with the highest temperature profile. This
experiment highlights the sensitivity of both melamine and formaldehyde migration to
minor variations in the contact temperature profile, even within the tolerable range.
Therefore, to accurately assess the stability of an article, it is crucial to conduct three
consecutive migrations with similar temperature profiles. This is essential to
avoid erroneously declarations of instability for an article that is in fact stable.

Challenges arise in maintaining consistent compliance statements concerning the SML,

as narrowing the tolerance range of the temperature in the food simulant may be
required. It should be noted that these observations may or may not be applicable to
other materials, articles, or migration conditions.

The EURL-FCM emphasises the critical importance of conducting migration tests strictly
under the required contact time and at the correct contact temperature of the food
simulant (not that of the oven). Based on appropriate analytical results and despite
acknowledging the complications to follow, the EURL challenges the tolerable range (70
± 2 oC) for the contact temperature laid down in the normative Annex C of EN 13130-
01:2004 [11], considering it too broad for some analytes (as melamine and
formaldehyde) under certain conditions (2 h at 70 oC) depending on the kinetic of the
migration process and thus insufficient to ensure comparable migration (Annex 9-10).

For future proficiency testing exercises involving a migration step, participants will be
requested to use exclusively calibrated data loggers capable of measuring the contact
temperature of the food simulant within the tested article at high frequency (30-60
seconds). Achieving a satisfactory profile requires thorough optimisation before the
actual migration experiment, using the spare article provided. When testing articles
repeatedly, laboratories must guarantee repeatable temperature profiles for the first,
second, and third migrations to ensure a proper assessment of migration stability. This
involves maintaining identical initial temperatures of the articles at the moment of filling
with the food simulant pre-heated to the same temperature.

Other factors that could impact migration, as demonstrated in the previous PTs, include
food simulant losses (up to 25 ml [13-15]) and their compensations, uniformity of the
contact temperature profile within the oven; timing and location of the food simulant
filling, accurate correlation between the measured volume and calculated contact
surface, etc. As a general guideline, the volume of the food simulant should be
measured at room temperature, while the contact surface should be calculated using a
mug filled with pre-heated food simulant.

6.3.6. Additional information extracted from the questionnaire

All participants completed the questionnaire, providing valuable information about their
laboratories, operational methodologies, and analytical methods. Annex 13 summarises
the experimental details, the technique used and additional information requested.
The majority of the participants (26 out of 43) were accredited according ISO 17025 for
the analyses of both melamine and formaldehyde in food simulants, while 10
participants are accredited only for formaldehyde and two exclusively for melamine. Six

20
participants declared that they do not have migration procedures within the scope of
their accreditation, and an additional five were not accredited for the scope of this PT.

Instrumental techniques applied

Analytical techniques for the analyses of melamine and formaldehyde in food simulant B
are presented in Table 4, while the additional experimental details are provided in Annex
13. The use of different instrumental techniques for both measurands did not impact the
performance of the laboratories in analysing test item 1, as shown in Annexes 5 and 6.

Table 4 Analytical techniques used to determine melamine (MEL) and formaldehyde

(FA) in test item 1.

Technique MEL FA
HPLC-DAD 3 1
HPLC-UV 13 7
LC-MS 17 1
LC-MS/MS 5 1
Spectrophotometry -- 23

The main difference among the instrumental techniques relates to the achievable Limits
of Quantification (LOQs). For melamine, reported LOQs start at 1 g kg-1 and higher for
LC-MS/MS, while for HPLC-UV they range from 1 to 1.5 mg kg-1, resembling reporting
limits more than LOQs. However, the majority of participants reported a reasonable LOQ
range of 0.05-0.5 mg kg-1. For formaldehyde, the LOQ range is much narrower (0.1-3
mg kg-1), and there is no significant difference observed based on the sample
preparation technique, whether using 2,4-dinitrophenylhydrazin, acetyl acetone or
chromotropic acid.

7 Conclusion
The proficiency test FCM-23/01 was organised to assess (i) the analytical capabilities of
EU National Reference Laboratories and Official Control Laboratories in determining the
mass fractions of melamine and formaldehyde in food simulant B and (ii) the ability to
assess the compliance of a repeated-use article against the new requirements outlined in
Commission Regulation (EU) 2020/1245.

The participants demonstrated a highly satisfactory overall performance in determining

these substances in food simulant B (3% acetic acid), with approximately 95 % of the
results achieving z scores below 2 (satisfactory) against the 15 % standard deviation for
proficiency assessment set by the EURL-FCM. This suggests that the pt could potentially
be further reduced in the future.

Most of the participants reported realistic measurement uncertainty estimations.

The task of evaluating participants' compliance statements regarding test item 2 posed
notable challenges as even minor variations in migration test conditions, while within
acceptable limits, significantly influenced the test results. Only 28% of the laboratories
accurately assessed compliance and stability for formaldehyde in test item 2, aligning
with the conclusions drawn by the European Reference Laboratory (EURL).

Assessing the stability of melamine and its compliance with the specific migration limit
(SML) for test item 2 proved to be particularly difficult as the migration was close to the

21
SML. Less than 20% of the laboratories correctly evaluated compliance and stability for
melamine in test item 2, consistent with the EURL conclusions.

In conclusion, the assessment of compliance for melamine-bamboo mugs remains a

challenging task that requires further investigation.
.

22
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with food, Official Journal of the European Union L 288/1 (2020). 32020R1245

[2] Commission Regulation, (EU) No 2017/625 of the European Parliament and of the Council
of 15 march 2017 on official controls and other official activities performed to ensure the
application of food and feed law, rules on animal health and welfare, plant health and plant
protection products, Official Journal of the European Union L 95/1 (2017). 32017R0625

[3] ISO/IEC 17043:2023 "Conformity assessment – General requirements for proficiency

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[6] SoftCRM, (n.d.). http://www.eie.gr/iopc/softcrm/index.html .

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[8] S L R Ellison and A Williams (Eds). Eurachem/CITAC guide: Quantifying Uncertainty in

Analytical Measurement, Third edition, (2012) ISBN 978-0-948926-30-3. Available from
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[9] Analytical Methods Committee, "MS EXCEL Add-in for Robust Statistics" and "Kernel
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[10] Commission Regulation (EU) No 10/2011 of 14 January 2011 on plastic materials and
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[11] EN 13130-1:2004 – “Materials and articles in contact with foodstuffs. Plastics substances
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[12] Analytical Methods Committee, "Representing data distributions with kernel density
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[13] Tsochatzis, E., Mieth, A., Simoneau, C., Hoekstra, E., Report of an inter-laboratory
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[14] Tsochatzis, E., J.F. Alberto Lopes, P. Robouch and E.J. Hoekstra; "EURL-FCM-02-2016
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[15] S. Valzacchi, J.L. Vicente, F. Cordeiro, P. Robouch and E.J. Hoekstra, "EURL-FCM-01-2017
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23
List of abbreviations and symbols
DAD Diode Array Detector
DG SANTE Directorate General for Health and Food Safety
EC European Commission
EFSA European Food Safety Authority
EU European Union
EURL European Union Reference Laboratory
FCM Food Contact Materials
GUM Guide for the Expression of Uncertainty in Measurement
GC-MS(MS/MS) Gas chromatography-mass spectrometry or tandem mass spectrometry
HPLC-FLD High performance liquid chromatography-fluorescence detection
HPLC-UV(DAD) High performance liquid chromatography-ultraviolet (diode array
detection)
ILC Interlaboratory Comparison
ISO International Organization for Standardization
JRC Joint Research Centre
LOD Limit of Detection
LOQ Limit of Quantification
NRL National Reference Laboratory
OCL Official Control Laboratory
PT Proficiency test
SOP Standard operating procedure

k coverage factor
pt standard deviation for proficiency test assessment
u(xi) calculated standard measurement uncertainty (of participant "i")
u(xpt) standard uncertainty of the assigned value
uchar (standard) uncertainty contribution due to characterisation
uhom (standard) uncertainty contribution due to homogeneity
ust (standard) uncertainty contribution due to stability
U(xi) reported expanded uncertainty by participant "i"
U(xpt) expanded uncertainty of the assigned value
xi reported mean value by participant "i"
xpt assigned value
z (or z') z (or z') score
 zeta score

24
List of figures

Figure 1: Overview of laboratory performance per measurand according to z and ζ

scores for formaldehyde and melamine in test item 1.

Figure 2: Box plots of the melamine and formaldehyde results reported by the
participants for three consecutive migrations from three mugs (MUG1-3).

List of tables

Table 1: Assigned values (xpt) and standard deviation for the PT assessment (σpt)
for melamine and formaldehyde in test item 1 (T1).

Table 2: Comprehensive presentation detailing compliance statements of the

participants related to MEL and FA, compliance assessed based on their
data, coherence of their statement to their data, the calculated relative
standard uncertainty, and the overall agreement with the EURL conclusions
(M and F for melamine and formaldehyde). In addition, the evaluation of the
temperature profile used for migration (S, Q, U, see migration conditions).

Table 3: Summarised overview of the compliance statements (for MEL and FA),
compliance assessed based on their data (stability and SML), corresponding
number of laboratories, coherence of their statement to their data,
agreement with the EURL conclusions

Table 4 Analytical techniques used to determine melamine (MEL) and formaldehyde

(FA) in test item 1.

25
A. Announcement of the PT round “FCM-23/01”

26
Annex 1: B. Invitation letter

27
Instructions for participants

28
29
30
Questionnaire

31
32
33
 Homogeneity and stability results

A. Homogeneity study for test item 1, all values in mg kg-1

test item 1
Melamine Formaldehyde
1 2.52 2.53 12.51 12.53
2 2.52 2.51 12.55 12.52
3 2.53 2.52 12.52 12.50
4 2.54 2.52 12.44 12.52
5 2.52 2.52 12.50 12.46
6 2.52 2.53 12.55 12.53
7 2.53 2.52 12.49 12.56
8 2.53 2.52 12.52 12.51
9 2.52 2.51 12.54 12.55
10 2.52 2.51 12.54 12.52
Mean 2.52 12.52
uhom 0.12 % 0.11 %
pt 15 % 15 %
0.3pt 4.5 % 4.5 %
uhom < 0.3 pt passed passed

Where: σpt is the standard deviation for the PT assessment,

uhom is the standard uncertainty contribution due to homogeneity

B. Homogeneity study for test item 2, all values in mg kg-1

Melamine Formaldehyde
MIG1 MIG2 MIG3 MIG1 MIG2 MIG3
Mug 1 3.36 3.53 3.79 9.51 10.20 10.99
Mug 2 3.41 3.34 3.19 9.29 10.10 10.86
Mug 3 3.34 3.67 3.97 9.13 10.89 12.06
Mug 4 3.08 3.49 3.65 8.84 10.19 10.97
Mug 5 3.99 3.81 3.76 8.42 9.34 9.42
Mug 6 3.85 3.05 3.62 8.35 7.86 9.37
Mug 7 3.35 3.67 3.82 9.92 11.13 11.80
Mug 8 3.17 3.06 3.20 7.80 8.91 9.63
Mug 9 3.70 3.18 3.40 10.02 10.62 10.91
Mug 10 3.20 3.39 3.66 8.59 10.12 10.86
Mean 3.45 3.42 3.61 8.99 9.94 10.69
RSD 8.8% 7.7% 7.3% 8.0% 9.9% 8.7%

34
C. Stability study at 40oC, 20oC and 4oC (RT) for one and/or 13 weeks
all values in mg kg-1 (REF, reference)
Melamine
T (°C) 4 °C (Ref.) 40 °C 20 °C 4 °C
weeks T0 1 13 13
2.52 2.53 2.52 2.53
2.52 2.52 2.53 2.53
2.53 2.51 2.53 2.53
2.53
2.52
2.53
2.52
2.53
2.51
2.52
Mean 2.52 2.52 2.53 2.53
|Y0-Yend| 0.001 0.003 0.007
0.3 pt 0.114
Stablea? yes yes yes

Formaldehyde
T (°C) 4 °C (Ref.) 40 °C 20 °C 4 °C
weeks T0 1 13 13
12.52 12.52 12.65 12.54
12.54 12.48 12.64 12.57
12.50 12.50 12.66 12.59
12.48
12.48
12.54
12.52
12.52
12.54
12.53
Mean 12.52 12.50 12.65 12.56
|Y0-Yend| 0.019 -0.132 -0.046
0.3 pt 0.563
Stablea? yes yes yes
a
Stability criteria according to ISO 13528:2022 § B.5. (|Y0-Yend| < 0.3 pt)

35
 Results for melamine in FS.B (test item 1)
Assigned range: xpt = 2.528 ± 0.0069 (k = 2 ); σpt = 0.379 , all values in mg kg-1

LabCode xi ± k Technique z score  score MU.

LN01 2.35 0.235 1.73 LC-MS -0.47 -1.31 a
LN02 2.45 21 2 LC-MS -0.21 -0.01 c
LN03 3.2 0.54 2 HPLC-UV 1.77 2.49 a
LN04
LN05 3.31 0.09 2 HPLC-UV 2.06 17.18 a
LN06
LN07 2.41 0.24 2 LC-MS -0.31 -0.98 a
LN08 2.54 0.61 2 LC-MS/MS 0.03 0.04 a
LN09 2.18 0.2 2 LC-MS -0.92 -3.47 a
LN10 2.61 0.65 2 LC-MS 0.22 0.25 a
LN11 2.44 0.49 2 LC-MS -0.23 -0.36 a
LN12 2.6 HPLC-UV 0.19 10.51 np
LN13 2.8 0.4 2 LC-MS/MS 0.72 1.36 a
LN14 2.45 0.32 2 HPLC-UV -0.21 -0.49 a
LN15 < 1.86 HPLC-UV
LN16 2.2 0.3 2 LC-MS -0.86 -2.18 a
LN17 2.51 0.12 2 HPLC-DAD -0.05 -0.30 a
LN18 2.81 0.12 2 HPLC-UV 0.74 4.67 a
LN19 0.026 0.0005 2 LC-MS -6.60 -364.40 a
LN20 2.65 1.06 2 LC-MS 0.32 0.23 c
LN21 2.42 0.65 1.73 HPLC-UV -0.28 -0.29 c
LN22
LN23 2.35 0.33 2 HPLC-DAD -0.47 -1.08 a
LN24 2.4 0.7 2 LC-MS/MS -0.34 -0.37 a
LN25 2.6 0.3 2 LC-MS 0.19 0.48 a
LN26 2.36 21 1.73 -0.44 -0.01 c
LN27 2.49 30 2 LC-MS -0.10 0.00 c
LO30 2.45 0.27 2 HPLC-UV -0.21 -0.58 a
LO31 2.57 1.14 1.64 LC-MS 0.11 0.06 c
LO32 2.5 LC-MS/MS -0.07 -4.07 np
LO33 2.53 0.506 2 HPLC-UV 0.01 0.01 a
LO34 2.4 0.6 2 LC-MS/MS -0.34 -0.43 a
LO35 2.42 HPLC-UV -0.28 -15.73 np
LO36 2.462 0.106 2 HPLC-DAD -0.17 -1.23 a
LO37 2.72 0.8 2 LC-MS 0.51 0.48 a
LO38 2.5 0.7 2 LC-MS -0.07 -0.08 a
LO39 2.54 1.27 2 HPLC-UV 0.03 0.02 c
LO40
LO43 2.42 0.68 2 HPLC-UV -0.28 -0.32 a
LO44 2.4 0.7 2 HPLC-UV -0.34 -0.37 a
LO45 2.39 0.24 2 LC-MS -0.36 -1.15 a
LO46
LO47 2.23 0.25 2 LC-MS -0.79 -2.38 a
LO48 2.7 20 2 LC-MS 0.45 0.02 c
Performance (z, ): Satisfactory (green); Questionable (yellow); Unsatisfactory (Red)
MU – “a” u(xpt,rel) ≤ u(xi,rel) ≤ σpt,rel ; “b” u(xi,rel) < u(xpt,rel); “c” u(xi,rel) > σpt,rel; “np” not provided

36
 5.00

FCM PT 23/01: Melamine in FS.B

4.50 xpt = 2.528 u(xpt) = 0.007  pt = 0.379 (in mg/kg)
(k=1) 'pt = SDPA z score
4.00
Mass fraction

3.50

3.00

2.50

2.00

1.50
HPLC-UV(DAD) LC-MS
LC-MS/MS
1.00
LN23

LN17
LN15

LN21
LN14

LN12
LN18
LN03
LN05
LN19
LN09
LN16

LN01

LN07
LN11
LN02
LN27

LN25
LN10
LN20

LN24

LN08
LN13
LN26
LN04
LN06
LN22
LO36

LO44
LO43
LO35

LO30
LO33
LO39

LO47

LO45

LO38
LO31

LO48
LO37

LO34
LO32

LO40
LO46
Laboratory Code
Measurement result ranges reported by participants
Assigned value (xpt): solid black line; Assigned range (xpt ± Upt (k=2)): dashed blue lines; Acceptance range (xpt ± 2 σpt): dotted red lines.

37
 Results for formaldehyde in FS.B (test item 1)
Assigned range: xpt = 12.48 ± 0.41 (k = 2); σpt = 1.87 (all values in mg kg-1)

LabCode xi ± k Technique z score  score MU.

LN01 13.35 2.67 1.73 Spectroph. 0.47 0.56 a
LN02 12.28 7.8 2 HPLC-UV -0.10 -0.05 c
LN03 11.45 0.99 2 Spectroph. -0.55 -1.91 a
LN04 11.8 2.87 2 Spectroph. -0.36 -0.47 a
LN05 12.54 0.13 2 Spectroph. 0.03 0.30 b
LN06 12.12 0.03 2 Spectroph. -0.19 -1.71 b
LN07 11.8 1.2 2 Spectroph. -0.36 -1.06 a
LN08 10.7 1.3 2 LC-MS/MS -0.95 -2.60 a
LN09 9.36 1.12 2 LC-MS -1.66 -5.22 a
LN10 12.42 2.48 2 Spectroph. -0.03 -0.04 a
LN11 12.4 1.9 2 Spectroph. -0.04 -0.08 a
LN12 14 HPLC-UV 0.81 7.37 np
LN13 12.4 1.7 2 Spectroph. -0.04 -0.09 a
LN14 11.75 0.94 2 Spectroph. -0.39 -1.41 a
LN15 1.15 0.23 2 Spectroph. -6.05 -47.85 a
LN16 12.1 1.4 2 Spectroph. -0.20 -0.51 a
LN17 12.57 0.79 2 Spectroph. 0.05 0.21 a
LN18 12.1 2.2 2 Spectroph. -0.20 -0.34 a
LN19 12.66 2.5 2 Spectroph. 0.10 0.15 a
LN20 11.96 0.84 2 HPLC-UV -0.28 -1.10 a
LN21 11.43 2.29 1.73 Spectroph. -0.56 -0.78 a
LN22 14.357 1.14 2 Spectroph. 1.01 3.10 a
LN23 12.6 1.9 2 Spectroph. 0.07 0.13 a
LN24 13 2 2 Spectroph. 0.28 0.51 a
LN25 10.8 0.8 2 Spectroph. -0.90 -3.72 a
LN26 12.32 7.81 1.73 -0.08 -0.03 c
LN27 10.1 10 2 Spectroph. -1.27 -0.47 c
LO30 11.66 1.68 2 HPLC-UV -0.44 -0.94 a
LO31 13.4 5.7 1.64 Spectroph. 0.49 0.27 c
LO32 12 Spectroph. -0.25 -2.30 np
LO33 13.28 2.656 2 HPLC-UV 0.43 0.60 a
LO34 11.4 1.7 2 HPLC-DAD -0.57 -1.23 a
LO35 12.53 1.23 2 Spectroph. 0.03 0.08 a
LO36 12.4 4 2 Spectroph. -0.04 -0.04 c
LO37 13 4.4 2 Spectroph. 0.28 0.24 c
LO38 11.3 2.3 2 Spectroph. -0.63 -1.01 a
LO39 11.6 2.57 2 HPLC-UV -0.47 -0.67 a
LO40 13.61 3.51 2 Spectroph. 0.61 0.64 a
LO43 12.88 2.81 2 Spectroph. 0.22 0.29 a
LO44 12 3 2 HPLC-UV -0.25 -0.31 a
LO45 11.9 1 2 Spectroph. -0.31 -1.06 a
LO46 13.3 2.1 2 Spectroph. 0.44 0.77 a
LO47
LO48 12 10.3 2 Spectroph. -0.25 -0.09 c
Performance (z, ): Satisfactory (green); Questionable (yellow); Unsatisfactory (Red)
MU – “a” u(xpt,rel) ≤ u(xi,rel) ≤ σpt,rel ; “b” u(xi,rel) < u(xpt,rel); “c” u(xi,rel) > σpt,rel; “np” not provided

38
 20.00
FCM PT 23/01: Formaldehyde in FS.B
18.00
xpt = 12.48 u(xpt) = 0.21  pt = 1.87 (in mg/kg)
(k=1) 'pt = SDPA z score

16.00
Mass fraction

14.00

12.00

10.00

8.00
LC-MS/MS

HPLC-UV(DAD) Spectrophotometry
6.00

4.00
LN20

LN02

LN12
LN09
LN08
LN15
LN27
LN25

LN21
LN03
LN14
LN04
LN07

LN16
LN18
LN06
LN11
LN13

LN10

LN05
LN17
LN23
LN19

LN24

LN01

LN22
LN26
LO34
LO39
LO30

LO44

LO33

LO38

LO45
LO32
LO48

LO36

LO35

LO43

LO37
LO46

LO31
LO40

LO47
Laboratory Code

Measurement result ranges reported by participants

Assigned value (xpt): solid black line; Assigned range (xpt ± Upt (k=2)): dashed blue lines; Acceptance range (xpt ± 2 σpt): dotted red lines.

39
 Repeated temperature profiles
(3 consecutive migrations between 68 and 72 oC (Profile 1)
performed by the EURL on a mug (test item 2)

Mig 1
73
High acceptability limit 72 °C
72
Temperature [°C]

71
70
69
68 Low acceptability limit 68 °C

67
0 50 100 150 200
Time [min]

Mig 2
73
High acceptability limit 72 °C
72
Temperature [°C]

71
70
69
68 Low acceptability limit 68 °C

67
0 50 100 150 200
Time [min]

Mig 3
73
High acceptability limit 72 °C
72
Temperature [°C]

71
70
69
68 Low acceptability limit 68 °C

67
0 50 100 150 200
Time [min]

40
Three different temperature profiles
within the recommended temperature range of 70 ± 2 oC,
obtained by the EURL for different mugs (test item 2)

68  T  72 oC

67.8  T  69.5 oC

67.5  T  68.3 oC

41
 Melamine results obtained by the EURL

A. Three consecutive migrations performed applying the same temperature

profile (see Annex 8, Profile 1). All migrations are above the SML; while
the reported ranges have overlapping uncertainties, demonstrating the
stability of the test item.

Melamine from bamboo mug (I-II-III MIG)

5.00
Expanded uncertainty from Horwitz
4.50
Migration mg kg-1

4.00

3.50

3.00

2.50

2.00
0 1 2 3 4
nth migration

B. First migrations of three different mugs performed at three different

temperature profiles (see Annex 8, Profiles 1, 2 and 3). Migrated levels
increase with increasing temperature ranges; those obtained for
temperatures ranging from 67.5 and 68.3 oC, are below the SML

42
 Formaldehyde migration results obtained by the
EURL

A. Three consecutive migrations performed applying the same

temperature profile (see Annex 7, Profile 1). All migrations are
below the SML; and the reported ranges have overlapping
uncertainties, demonstrating the stability of the test item.

B. First migrations of three different mugs performed at three different

temperature profiles (see Annex 8, Profiles 1, 2 and 3). Migrated
levels increase with increasing temperature ranges.

Formaldehyde from bamboo cup (1st migration only) 68-70-72 °C

16.00

14.00

12.00
Migration, mg kg-1

10.00

8.00 
6.00


4.00

2.00
67 68 69 70 71 72 73
simulant temperature @ 120 min

43
 Reported results for three consecutive migrations (m1, m2, m3) of melamine in food
simulant B from test item 2 (MUG), expressed in mg kg-1

T profile
MUG 1 MUG 2 MUG 3
U(m1) Rsu U(m1) Rsu U(m1) RSu
Lab m1 m2 m3 k=2 k k=1 m1 m2 m3 k=2 k k=1 m1 m2 m3 k=2 k k=1 Lab statement Stable < SML coherent
LN01 2.41 2.43 2.72 0.241 1.73 5.8% 2.05 2.11 2.26 0.205 1.73 5.8% 2.59 2.83 2.9 0.259 1.73 5.8% NC yes no yes S
LN02 2.24 2.31 2.37 0.235 1 10.5% 2.41 2.41 2.2 0.253 1 10.5% 1.9 2.3 2.39 0.200 1 10.5% C yes yes yes Q
LN03 1.09 1 0.85 0.17 2 7.8% 1.16 1.53 1.07 0.21 2 9.1% 1.05 1.18 0.91 0.17 2 8.1% C yes yes yes U
LN04 -- not tested U
LN05 2.803 2.826 3.528 np 3.086 3.748 3.424 np 4.037 3.047 3.822 np NC ? ? ? S
LN06 -- not tested S
LN07 2.13  2.63 2.6 0.26 2 6.1% 2.05 2.2 2.01 0.25 2 6.1% 1.95 2.33 2.01 0.23 2 5.9% NC no yes yes S
LN08 2.07 1.88  2.96 0.5 2 12.1% 1.4 1.46  2.45 0.34 2 12.1% 1.82 2.02 2.8 0.44 2 12.1% NC no yes yes Q
LN09 1.25 0.63  0.73 0.08 2 3.2% 1.07 0.88 0.99 0.09 2 4.2% 0.99 0.71  0.9 0.08 2 4.0% C no yes no U
LN10 1.6 1.6 1.9 0.41 2 12.8% 2.3 2 2.3 0.58 2 12.6% 1.6 1.3 1.5 0.4 2 12.5% C yes yes yes U
LN11 2.12 2.62 3 0.43 2 10.1% 2.61 2.62 3.2 0.53 2 10.2% 1.82 1.8 2.13 0.37 2 10.2% NC yes no yes U
LN12 1.4 2.2 1.8 np 1.6 1.6 2.1 np 1.9 1.6 2 np C ? yes ? Q
LN13 3.4 3.3 3.6 1 2 15% 3.1 2.7 3.2 0.9 2 15% 3.8 3.3 3.5 1.1 2 14.5% NC yes no yes S
LN14 2.76 2.43 2.82 0.75 2 13.6% 3.24 2.97 3.22 0.86 2 13.3% 3.17 3.1 3.36 0.85 2 13.4% NC yes no yes Q
LN15 < 1.86 < 1.86 < 1.86 np < 1.86 < 1.86 < 1.86 np < 1.86 < 1.86 < 1.86 np NC yes yes no S
LN16 1.4 0.4 < 0.25 0.2 2 7.1% 0.9 0.3 < 0.25 0.1 2 5.6% 1 0.4 0.3 0.1 2 5.0% C yes yes yes
LN17 0.95 0.35  1.37 0.05 2 2.6% 1.05 0.28  1.48 0.06 2 2.9% 0.83 0.58  1.28 0.05 2 3.0% NC no yes yes Q
LN18 3.39 3.17 2.89 0.3 2 4.4% 3.37 3.21 2.81 0.29 2 4.3% 3.68 3.07 2.74 0.32 2 4.3% NC yes no yes S
LN19 0.92 0.78 0.63 0.19 2 10.3% 0.77 1.06 0.84 0.15 2 9.7% 1.27 0.96 0.74 0.25 2 9.8% C yes yes yes
LN20 1.05 1.25 1.24 0.42 2 20% 1.84 2.15 2.09 0.74 2 20% 1.72 1.91 1.99 0.69 2 20% C yes yes yes S
LN21 4.39 2.85 3.51 0.97 1.73 12.8% 3.11 2.44 4.2 0.88 1.73 16.4% 5.36 4.54 5.45 1.38 1.73 15% NC yes no yes U
LN22 -- not tested
LN23 1.85 1.61  2.38 0.26 2 7.0% 1.41 1.84 1.83 0.28 2 9.9% 1.86 2.1  2.8 0.3 2 8.1% NC no yes yes S
LN24 1.8 1.6 2.4 0.6 2 17% 2.5 2.8 2.6 0.9 2 18% 1.3 2.3 1.9 0.5 2 19% C yes yes yes S
LN25 2.8 2.5 2.9 0.3 2 5.4% 2.5 2.4 2.6 0.2 2 4.0% 2.9 2.3 2.1 0.3 2 5.2% NC yes no yes S
LN26 0.69  2.16 2.34 0.07 1.73 6.1% 0.77  1.89  2.63 0.08 1.73 6.1% 0.54  2.43 2.43 0.06 1.73 6.1% NC no yes yes S
LN27 3.23 2.88 2.95 0.969 2 15% 1.75 2.08 2.08 0.525 2 15.0% 2.71 3.2 3.12 0.813 2 15.0% C yes yes yes S
LO30 1.63  2.71 2.87 0.18 2 5.5% 1.09  2.02 2.01 0.12 2 5.5% 2.02  2.77 2.88 0.22 2 5.4% NC no no yes S
LO31 1.7 1.9 2.42 0.75 1.64 27% 2.31 2.52 0.92 1.03 1.64 27% 2.07 1.55 1.61 0.92 1.64 27% C yes yes yes S
LO32 3.3 2.3 2.9 np 3.4 3.8 3.6 np 2.3 3.7 3.5 np NC ? ? ? S
LO33 1.75 2.15 1.71 np 1.54 2.01 1.5 np 1.03 1.47 1.64 np C ? yes ? S
LO34 2.2 2.6 3.1 0.6 2 13.6% 2.2 2.3 2.8 0.6 2 13.6% 2.5 2.4 2.6 0.6 2 12.0% C yes yes yes S
LO35 1.55 1.82 1.76 np 1.86 1.64 1.94 np 1.52 1.32 1.39 np C ? yes ? Q
LO36 1.559 1.717 1.919 0.67 2 21% 1.718 1.553 1.67 0.739 2 22% 1.557 1.67 1.869 0.67 2 22% C yes yes yes U
LO37 2.03 1.73 2.35 0.6 2 15% 2.22 2.2 2.99 0.65 2 15% 1.52 1.68 2.24 0.45 2 15% NC yes yes no Q
LO38 0.6 0.5 0.5 0.2 2 17% 0.8 0.9 0.7 0.3 2 19% 1.2 1 0.9 0.4 2 17% C yes yes yes Q
LO39 1.03 0.94 1.42 0.52 2 25% 1.18 1.12 1.26 0.59 2 25% 1.72 1.38 1.48 0.86 2 25% NC yes yes no S
LO40 -- not tested Q
LO43 2.21 1.93 1.88 0.63 2 14.3% 1.56 1.88 1.79 0.47 2 15% 1.32  2.39 2.27 0.41 2 16% NC no yes yes S
LO44 0.9 0.8 1.3 0.3 2 17% 0.9 0.9 1.3 0.3 2 17% 0.8 1 1 0.2 2 12.5% NC yes yes no Q
LO45 1.77 1.8 1.8 0.18 2 5.1% 1.29 1.23 1.34 0.13 2 5.0% 1.8 1.83 1.97 0.19 2 5.3% C yes yes yes S
LO46 -- not tested
LO47 4.5 3.09 2.76 0.49 2 5.4% 4.89  13.39 5.26 0.54 2 5.5% 4.3  5.77 2.5 0.47 2 5.5% NC no no yes S
LO48 1.2 1.6  2.9 0.24 2 10.0% 1.1  1.8 2.5 0.22 2 10.0% 1.3  2.3 2.8 0.26 2 10.0% NC no yes yes S

44
 Reported results for three consecutive migrations (m1, m2, m3) of formaldehyde in
food simulant B from test item 2 (MUG), expressed in mg kg-1
MUG 1 MUG 2 MUG 3

T profile
U(m1) RSD U(m1) RSD U(m1) RSD
Lab m1 m2 m3 k=2 k k=1 m1 m2 m3 k=2 k k=1 m1 m2 m3 k=2 k k=1 Lab statement Stable < SML coherent
LN01 8 9.28 10.12 1.6 1.73 11.6% 6.77 7.68 8.64 1.35 1.73 11.5% 7.44 8.92 9.57 1.49 1.73 11.6% C yes yes yes S
LN02 6.54  7.9 7.9 0.26 1 3.9% 9.45  10.81 10.62 0.37 1 3.9% 7.99  9.78 10.43 0.31 1 3.9% NC no yes yes Q
LN03 3.22 2.48 2.4 0.39 2 6.1% 2.62  4.21 2.58 0.46 2 8.8% 2.6  3.47 1.79 0.38 2 7.3% C no yes no U
LN04 1.686 1.548  2.014 0.257 2 7.6% 1.329 1.334 1.765 0.257 2 9.7% 1.828 1.231  1.889 0.257 2 7.0% NC no yes yes U
LN05 3.686 7.334 7.131 np 5.826 11.744 9.904 np 6.892 11.563 9.941 np NC ? yes ? S
LN06 3.945 7.423 7.357 np 5.716 12.61 10.026 np 6.177 10.966 10.639 np NC ? yes ? S
LN07 6.2  8.7 9.3 0.8 2 6.5% 6  7.9 8 0.8 2 6.7% 5.5  7.6 7.5 0.7 2 6.4% NC no yes yes S
LN08 6.71 7.81  11.2 0.8 2 6.0% 3.52  4.33  6.43 0.42 2 6.0% 6.28 7.47  9.62 0.75 2 6.0% NC no yes yes Q
LN09 3.29 2.24  3.92 0.38 2 5.8% 3.48 3.71 3.5 0.43 2 6.2% 2.34 2.41 2.8 0.3 2 6.4% C no yes no U
LN10 5.7 6 3.6 1.1 2 9.6% 6.9 6.7 4.4 1.4 2 10.1% 7.7 7.3 5 1.5 2 9.7% C yes yes yes U
LN11 7.4  10.1 10.8 1.2 2 8.1% 8 9.2 6.3 1.2 2 7.5% 4.6 5.7  9.8 0.7 2 7.6% NC no yes yes U
LN12 3.2 5.3 6.6 np 5.2 5.7 6 np 6.1 5.9 6.8 np C ? yes Q
LN13 10.9 11.4 11.7 3.1 2 14% 8.1 8.3 8.4 2.3 2 14% 11.4 12.2 12.2 3.3 2 14% C yes yes yes S
LN14 8.2 9.75 10.8 1.9 2 11.6% 7.12 7.86 8.69 1.69 2 11.9% 9.3 10.95 11.75 2.12 2 11.4% C yes yes yes Q
LN15 1.73 1.8 1.82 0.36 2 10.4% 1.62 1.89 1.56 0.34 2 10.5% 1.64 1.95 1.64 0.35 2 10.7% NC yes yes no S
LN16 4.6 <3 <3 0.5 2 5.4% 3.1 <3 <3 0.4 2 6.5% <3 <3 <3 C yes yes yes
LN17 3.9 2.35  6.38 0.53 2 6.8% 3.9 1.88  6.53 0.53 2 6.8% 3.43 3.59  6.22 0.53 2 7.7% NC no yes yes Q
LN18 12.6 13.8 12.6 2.5 2 9.9% 11.4 12.6 11.4 2.3 2 10.1% 9.6 10.8 9.6 1.9 2 9.9% C yes yes yes S
LN19 1.78  2.54 2.81 0.35 2 9.8% 2.66  5.45 3.51 0.52 2 9.8% 2.44  4.46 2.89 0.48 2 9.8% C no yes no
LN20 2.83 4.11 4.28 0.85 2 15% 6.44 8.77 8.72 1.93 2 15% 5.85 8.49 8.16 1.76 2 15% C yes yes yes S
LN21 9.33 8.69 9.89 1.86 1.73 11.5% 6.44 7.48 11.2 1.67 1.73 15.0% 13.91 15.18 16.49 3.04 1.73 12.6% C yes yes yes U
LN22 23.10 11.44 8.51 1.14 2 2.5% 11.44 4.81  8.38 1.14 2 5.0% 15.28 11.31 8.63 1.14 2 3.7% -- no yes U
LN23 9.6 10.5 11.3 3.6 2 19% 7.4 8.2 8.8 3.5 2 24% 10.2 10.9 12.4 4.6 2 23% NC yes yes no S
LN24 4.6 5.8 4.9 1.1 2 12.0% 8.1  12 11 1.9 2 11.7% 3  7.8 5.8 0.72 2 12.0% NC no yes yes S
LN25 8.6 8.6 9.4 0.6 2 3.5% 6.4 6.6 7.4 0.6 2 4.7% 9 8.8 8.8 0.7 2 3.9% C yes yes yes S
LN26 1.33  6.01  7.4 0.05 1.73 2.3% 1.31  4.62  6.32 0.05 1.73 2.3% 1.67  7.24  7.9 0.07 1.73 2.3% NC no yes yes S
LN27 6.56  7.85 7.9 0.656 2 5.0% 4.69  5.8 5.37 0.469 2 5.0% 8.2  10.2 9.88 0.82 2 5.0% C no yes no S
LO30 5.67  9.33 9.57 0.82 2 7.2% 3.41  5.91 6.77 0.49 2 7.2% 4.94  10.44 10.81 0.71 2 7.2% NC no yes yes S
LO31 6.64 8.7 7.46 2.86 1.64 26% 7.37 9.04 4.35 3.17 1.64 26% 7.29 8.48 6.95 3.13 1.64 26% C yes yes yes S
LO32 11.6 9.4 10.8 np 10.6 12.1 11.9 np 7.8 11.6 11.3 np C ? yes ? S
LO33 6.029 7.86 7.346 np 5.467 6.633 5.441 np 4.49 5.07 7.057 np NC ? yes ? S
LO34 7.6 9.5 9.6 1.1 2 7.2% 8.4 8.7 10.2 1.3 2 7.7% 8.9 9.8 10.8 1.3 2 7.3% C yes yes yes S
LO35 5.88  7.49 7.12 0.6 2 5.1% 3.82  4.92 5.62 0.4 2 5.2% 3.92  5.01 5.35 0.4 2 5.1% C no yes no Q
LO36 6.6 8 8.3 2.1 2 16% 6.6 7.9 8.4 2.1 2 16% 6.6 7.9 8.3 2.1 2 16% C yes yes yes U
LO37 7 8 10 2.4 2 17% 7 8 10 2.4 2 17% 5 6 7 1.68 2 17% NC ? yes ? Q
LO38 2 2.2 3.2 np 2 2.7 3.3 np 2 2 2.4 np NC ? yes ? Q
LO39 3.26 4.06 4.88 0.87 2 13.3% 3.59 4.12 4.85 0.95 2 13.2% 5.31 5.98 4.84 1.32 2 12.4% NC yes yes no S
LO40 1.39  3.27 2.45 0.5 2 18% 1.25  2.9 2.31 0.46 2 18% 2.05 3.41 2.29 0.66 2 16% NC no yes yes Q
LO43 9.24 10.01 10.44 2.1 2 11.4% 6.41 8.38 8.21 1.55 2 12.1% 5.74  10.54 10.12 1.41 2 12.3% NC no yes yes S
LO44 4.4 4.7  7.6 0.9 2 10.2% 2.4  3.6 4.7 0.5 2 10.4% 4.3 5.2 5.2 0.9 2 10.5% NC no yes yes Q
LO45 5.3 6.1 6.3 0.5 2 4.7% 4.5 5 5.2 0.4 2 4.4% 5.2  6.1 6.6 0.5 2 4.8% NC no yes yes S
LO46 7.58 5.74  10.1 1.7 2 11.2% 11.4 8.88  14 2.4 2 10.5% 11 8.05  12.5 2.1 2 9.5% C no yes no
LO47 -- -- -- not tested
LO48 10  12 14 1.03 2 5.2% 7  9 9 0.721 2 5.2% 9  13 12 0.927 2 5.2% NC no yes yes S

45
Results of the questionnaire

46
LC Code Laboratory Compliance Justification Compliance Justification Accreditation for
status statement statement melamine and
regarding regarding formaldehyde in
melamine formaldehyde food simulant B?

LN01 NRL non compliant The third test of mug 3 gave a result of 2,90 ± 0,290 mg/kg melamine (FCM No. 239) compliant The apparent increase in formaldehyde migration from the first to the second and third migration Yes, for both
and is above the specific migration limit of 2,5 mg/kg food or simulant given in the result in all mugs is insufficiently verifiable with the given measurement uncertainty. Therefore,
union list. Therefore, the whole test item 2 is non-compliant. for official control, non-compliance cannot be proven based on these results. However, from the
point of view of the BO, compliance cannot be proven either!

LN02 NRL compliant M1>M2; M2>M3 and M1>M3 ; M3<SML non-compliant M2>M1 and M3>M1; Yes, for both

LN03 NRL compliant (1) The mean levels of migration from test Item 2 (from all 3 mugs) in mg/kg are as compliant (1) The mean levels of migration from test Item 2 (from all 3 mugs) in mg/kg are as follows: MIG1 Yes, for both
follows: MIG1 = 1.10 ± 0.18; MIG2 = 1.24 ± 0.21; MIG3 = 1.02 ± 0.17. All of them are = 2.81 ± 0.41; MIG2 = 3.39 ± 0.0.50; MIG3 = 2.26 ± 0.32. All of them are below the SML (15
below the SML (2.5 mg/kg). (2) Migration is above the LOD in any of the three mg/kg). (2) Migration is above the LOD in any of the three migration tests; MIG1 < MIG2 > MIG3;
migration tests; MIG1 < MIG2 > MIG3; MIG2 is not significantly higher than MIG1 (zeta MIG2 is not significantly higher than MIG1 (zeta < 2); the stability of the material is sufficient.
< 2); the stability of the material is sufficient.
LN04 NRL compliant Melamine is not measured. non-compliant Migration 3 is bigger than migration 2. Yes, for FA

LN05 NRL, OCL non compliant MIG3>SML and "Insufficient Stability" e.g. MIG2>MIG1 or/and MIG3>MIG2 or/and non-compliant Although MIG3<SML the Stability of the Material is Insufficient. MIG2>MIG1 and Yes, for FA
MIG3>MIG1 MIG1<MIG3<MIG2
LN06 NRL, OCL non compliant MIG3>SML and "Insufficient Stability" e.g. MIG2>MIG1 or/and MIG3>MIG2 or/and non-compliant Although MIG3<SML the Stability of the Material is Insufficient. MIG2>MIG1 and Yes, for FA
MIG3>MIG1 MIG1<MIG3<MIG2
LN07 NRL non compliant The stability of the material shall be considered insufficient. The second migration test non-compliant The stability of the material shall be considered insufficient. The second migration test exceeds Yes, for MEL;
exceeds the level observed in the first test - MIG1 < MIG2. the level observed in the first test - MIG1 < MIG2. The third migration test is approx. at the same
level observed in the second test.
LN08 NRL non compliant Compliant with SML but non compliant with requirement of stability of material. non-compliant Compliant with SML but non compliant with requirement of stability of material. Migration tests Yes, for both
Migration test of cup 2 resulted in non compliance with stability. See used rule under of all three cups resulted in non compliance with stability. See used rule under point 22.
point 22.

LN09 NRL, OCL compliant Result below SML. Stability OK. M3>M2 but not significantly when taking MU into compliant Result below SML. Stability OK. M3>M2 but not significantly when taking MU into account Yes, for FA
account
LN10 NRL compliant the amount of migration and stability are ok compliant the amount of migration and stability are ok Yes, for both
LN11 NRL non compliant The third migration for the second mug is over the SML of 2.5 mg/kg (3.20 +/- 0.64 non-compliant The stability is insufficient for mugs 1 and 3 : the migration increases between the first and third Yes, for FA
mg/kg) tests (mug 1: 7.4 +/- 1.2 < 10.8 +/- 1.7 - mug 3: 4.6 +/- 0.7 < 9.0 +/- 1.4)

LN12 NRL compliant the values are stable and under the specific migration limit compliant the values are stable and under the specific migration limit Yes, for both

LN13 NRL non compliant MIG3>SML for 2 out of 3 mugs -> non-compliant. Compliant acc. to stability rule. compliant MIG3<SML and compliant acc. to stability rule. Yes, for both
Applying lab’s MU instead of Horwitz would result in compliant mugs.

LN14 NRL non compliant The migration of melamine in the 3rd migration test was found to exceed the SML of compliant For all the subsamples tested: The migration of formaldehyde in the 3rd migration test was lower Yes, for both
2.5 mg/kg for 2 out of the 3 subsamples tested. The relevant criterion for non- than the SML of 15 mg/kg. The migration from the first to the third migration test did not
compliance is: (m3 - SML )/[(u(m3)] > 1.64. The Horwitz equation was used to increase significantly. Regarding the stability of the material, the criterion for compliance is: (mj -
calculate the measurement uncertainty. mi )/[(u(mj) + u(mi)] < 1.64. The Horwitz equation was used to calculate measurement
uncertainties.
LN15 NRL non compliant The result is below our LOQ value, LOQ is1,86mg/kg. Formaldehyde leaching stability non-compliant M1>M2<M3 Yes, for both
of the sample: M1>M2<M3

47
LC Code Laboratory Compliance Justification Compliance Justification Accreditation for
status statement statement melamine and
regarding regarding formaldehyde in
melamine formaldehyde food simulant B?
LN16 NRL compliant Sample complies with Commission Regulation (EU) 2020/1245 as their is no increase compliant Sample complies with Commission Regulation (EU) 2020/1245 as their is no increase between Yes, for both
between extractions extractions

LN17 NRL non According to Reg (EU) 2020/1245 the samples are not compliant because MIG3 is non- According to Reg (EU) 2020/1245 the samples are not compliant because MIG3 is higher than Yes, for both
compliant higher than MIG2 and MIG1 compliant MIG2 and MIG1

LN18 NRL non compliant The stability of the material is sufficient because in any of the three migration tests, compliant The stability of the material is sufficient because in any of the three migration tests, the migration Yes, for FA
the migration does not increase from the first migration test to the third migration test does not increase from the first migration test to the third migration test (mx+1 – mx > 1.64
(mx+1 – mx > 1.64 ( x+1+ x) → (m(x+1) - m(x)) / (u(x+1)+u(x)) < 1.64), and the specific ( x+1+ x) → (m(x+1) - m(x)) / (u(x+1)+u(x)) < 1.64), and the specific migration limit is not
migration limit is exceeded in the third test (m3 – 1.64 u3) > ML →((m3 – ML) / exceeded in the third test (m3 – 1.64 u3) > ML → ((m3 – ML) / u3 < 1.64).
𝑢 𝑢 𝑢 𝑢
u3 > 1.64).
LN19 NRL compliant below MRL and no increase compliant below MRL and no increase Yes, for both

LN20 NRL compliant All migrations for all 3 mugs are below 2.5 mg/kg compliant All migrations are below 15 mg/kg Yes, for FA

LN21 NRL non compliant Because the average of the 3 MUGs for MIG3 > SML + U compliant Because the average of the 3 MUGs for MIG3 < or = SML+U; also there are no statistically No
differences between averages of MIG1 and MIG2, MIG2 and MIG3, MIG1 and MIG3

LN22
LN23 NRL non compliant Item 2 doesn´t meet requirements according Commission Regulation (EU) 2020/1245 - non-compliant Item 2 doesn´t meet requirements according Commission Regulation (EU) 2020/1245 - Annex V Yes, for FA
Annex V Chapter 2 - 2.1.6. Chapter 2 - 2.1.6.

LN24 NRL compliant m3 < SML (Mug 1 and 3) and m3 < SML for Mug 2 taking into account our own non-compliant m3 < SML, but INSUFFICIENT STABILITY: Mug 1: m3 > m1 and m3 > m2, Mug 3: m3 >m1 and m2 > No
laboratory expanded MU (2.6±0.9mg/kg) or using the statistical tool from draft JRC m1 using the statistical tool from draft JRC 2022 document, point 3.3.b). Using our own
document ''Options for checking compliance ..2022'', point 3.3 a). Stability rule: m1 > laboratory expanded MU: Mug 1: m3 > m1, Mug 3: m3 >m1 and m2 > m1; slightly different
m2 and m2 > m3 and m1 > m3, taking into account our own laboratory expanded MU interpretation but still not compliant sample.
or using the statistical tool from draft JRC document, point 3.3.b).

LN25 NRL non compliant Result in MUG1 MIG3-U (2.6 mg/kg) > SML (2.5 mg/kg). compliant Results in MUG1, MUG2 and MUG3 MIG3-U <= SML (15 mg/kg) and stability rule is compliant. Yes, for both

LN26 NRL non compliant Taking into account cup 2-4 since cup 1 cracked during migration. Cup 2: M2>M1, non-compliant Taking into account cup 2-4 since cup 1 cracked during migration. M2>M1, M3>M2, M3>M1 No
M3>M1; Cup 3: M2>M1, M3>M1; Cup 4: M3>SML, M2>M1, M3>M1
LN27 NRL compliant all 3 mugs tested: non-significant increase because all values for migration 1, 2 and 3 compliant mug 2 and mug 3: significant increase between migration 1 and 2, but non-significant increase for Yes, for both
within measurement uncertainty (±30 %). all 3 mugs tested: SML not exceeded mug 1, increase remains within measurement uncertainty (±30 %)
considering the measurement uncertainty of ±30 %

LO30 OCL non compliant According to the stability rule none of them are compliant. Based on the MIG3, only non-compliant Not compliant neither according to the stability rule but compliant if only the 15 mg/kg SML on Yes, for both
MUG2 is compliant. MUG1 is about 2.56 mg/kg (considering the Uc) and MUG3 about the MIG3 is considered.
2.57
LO31 OCL compliant Taking into account the measurement uncertainty, the values are below the limit value compliant Taking into account the measurement uncertainty, the values are below the limit value or there is Yes, for both
or there is no increase in migration. no increase in migration.
LO32 other non compliant migrationlimit for melamine according to regulation (EU) No 10/2011 exceeded. compliant migrationlimit for melamine according to regulation (EU) No 10/2011 not exceeded, partially Yes, for both
Partially increase in migration from first to third test but not consistent. Significance increase in migration from first to third test but not consistent. Significance questionable, stability
questionable, stability is classified as compliant. is classified as compliant.

48
LC Code Laboratory Compliance Justification Compliance Justification Accreditation for
status statement statement melamine and
regarding regarding formaldehyde in
melamine formaldehyde food simulant B?
LO33 other compliant below the SML; stability of the material pass non- Below the SML but - Stability test of the materilas fail. Yes, for both
compliant

LO34 OCL compliant SML: Migration values are exceeding the SML of 2.5 mg/kg in the 3rd migration test of compliant SML: Migration values are below the SML of 15 mg/kg in the 3rd migration test of each mug; Yes, for both
each mug. However, the exceedance is not statistically significant due to the Stability rule: Migration values are generally increasing for each mug. However, the increase is
measurement uncertainty of the method (25 %) and the criteria by Horwitz; Stability not statistically significant due to the criteria by Horwitz.
rule: Migration values are generally increasing for each mug. However, the increase is
not statistically significant due to the criteria by Horwitz.
LO35 OCL compliant result MIG3 below SML 2,5 mg/kg compliant result MIG3 below SML 15 mg/kg Yes, for both

LO36 OCL compliant compliant taking into account the expanded measurement uncertainty (including compliant compliant taking into account the expanded measurement uncertainty Yes, for both
measurement uncertainty of the migration)

LO37 other non compliant insufficient stability: compliance of the material is not be established even the specific non-compliant insufficient stability: compliance of the material is not be established even the specific migration Yes, for both
migration limit is not exceeded in any of the three tests (value of migration for third limit is not exceeded in any of the three tests
test of MUG2 is compliant with the uncertainty).
LO38 OCL compliant non-compliant There is a significant increase in formaldehyde concentration in the three attacks Yes, for both

LO39 OCL non compliant The requirement reported on Reg EU 10/2010 (point 2.1.6) is not satisfied. For MUG1, non-compliant The requirement reported on Reg EU 10/2010 (point 2.1.6) is not satisfied. For MUG1 e MUG2: Yes, for both
MUG2 and MUG3: MIG3 level exceeds MIG2 level. MIG2 level exceeds MIG1 level and MIG3 level exceeds MIG2 level. For MUG3: MIG2 level
exceeds MIG1 level.
LO40 other non compliant test not performed non-compliant Specific Migration (MS) is less than LMS sed the sample is not stable: MIG3<LMS, MIG3<MIG2 e No
MIG2>MIG1
LO43 OCL non compliant Even if the specific migration limit is not exceeded in any of the three tests, the result non-compliant Even if the specific migration limit is not exceeded in any of the three tests, the result is not No
is not compliant because an increase from the first migration test to the third compliant because an increase from the first migration test to the third migration test is
migration test is observed, indicating an insufficient stability of the material. observed, indicating an insufficient stability of the material.
LO44 other non compliant sample unstable non-compliant sample unstable Yes, for both

LO45 OCL compliant The value at the third incubation for all mugs are <LMR and all the mugs are stable non-compliant The value at the third incubation for all mugs are <LMR but the mug 2 is not stable for second Yes, for both
incubation compare to the first incubation
LO46 OCL non compliant We not test the item compliant All determinations have a value less than 15 mg/kg Yes, for FA

LO47 OCL non compliant Concentration for 3 mugs over SML non-compliant No analyzed Yes, for MEL;

LO48 other non compliant MIG 3 is >SML (MUG 1 and MUG 3), and the samples are not stable as migration non-compliant Although the results obtained are <SML, the sample is not stable as migration increases with Yes, for FA
increases with contacts (the rule (mj-mi)/[MU(mj)+MU(mi)]>1.64 (uncertainty K=1) contacts (the rule (mj-mi)/[MU(mj)+MU(mi)]>1.64 (uncertainty K=1) has been used as a criterion
has been used as a criterion for stability assessment). for stability assessment).

49
LC Code Accreditation Please specify Did you pre-heat Temperature of the How did you control the Did you Volume of the food Temperature of the food Did you measure If yes, please report the Analytical
for the the simulant food simulant temperature of the food preheat the simulant used for the simulant during the migration the food volume of the losses in ml techniquecs
migration before filling the before filling of the simulant during the mugs before migration experiments experiment (in oC) simulant losses for melamine
procedure? artide? test items migration experiments migration?

LN01 no YES 80 °C calibrated datalogger No 410 ml will be sent via mail Yes MUG 1: 8.3, 7.8, 7.0 ml LC-MS/MS
|| MUG 2: 7.8, 7.5, 5.3
ml || MUG 3: 5.5, 6.1,
7.0 ml

LN02 yes YES 75 °C calibrated datalogger No 420 ml See excel file attached Yes No loss HPLC-UV

LN03 yes EN 1186-3:2022 YES 72 °C non-calibrated No 400 ml 70.1 +/- 1.0 oC Yes 5 ml HPLC-UV
thermometer/datalogger

LN04 no YES 75 °C calibrated thermometer Yes 400 ml No HPLC-UV

LN05 yes YES 85 °C non-calibrated No 430 ml 70.1-71.9 oC No HPLC-UV

thermometer/datalogger
LN06 yes YES 85 °C non-calibrated No 430 ml 70.1-71.9 oC No HPLC-UV
thermometer/datalogger
LN07 yes YES 73 °C non-calibrated Yes 470 ml Yes 10 ml LC-MS/MS
thermometer/datalogger

LN08 yes YES 72 °C calibrated thermometer No 450 ml Sent by email Yes Weight of simulant was LC-MS/MS
measured after migration
and used for further
calculation of result

LN09 no We have validated the YES 70 °C calibrated datalogger No 445 ml Yes 1 LC-MS/MS
procedure
LN10 yes YES 73,5 °C calibrated datalogger No 470 ml No LC-MS/MS
LN11 yes YES 78 °C calibrated datalogger No 470 ml No LC-MS/MS

LN12 yes yes by the COFRAC YES 70°C calibrated datalogger No 400 ml No HPLC-UV

LN13 no - YES 72.3 calibrated datalogger Yes 430 ml MIG1: 69.7-71.2 °C / MIG2: Yes 7-12 mL LC-MS/MS
69.8-71.3 °C / MIG3: 69.1-
70.8 °C

LN14 yes YES 72°C calibrated thermometer No 450 ml Temperature range: 67.5°C - No HPLC-DAD
70.0°C

LN15 yes Melamine: CEN/TS 13130- YES 70°C calibrated thermometer No 450 ml send by mail Yes 3,5mL HPLC-UV
27:2005, Formaldehyde: MSZ
EN ISO 4614-2000(B)

50
LC Code Accreditation Please specify Did you pre-heat Temperature of How did you control the Did you Volume of the food Temperature of the food Did you If yes, please report the Analytical
for the the simulant the food simulant temperature of the food preheat the simulant used for the simulant during the measure the volume of the losses in techniquecs
migration before filling the before filling of simulant during the mugs before migration experiments migration experiment (in oC) food simulant ml for melamine
procedure? artide? the test items migration experiments migration? losses
LN16 yes YES 70 oC Other (please specify) No 475 ml 70oC No LC-MS/MS

LN17 no YES 70 °C calibrated datalogger No 450 ml 70 °C No HPLC-DAD

LN18 yes YES 72 °C calibrated datalogger No 453 ml 70±2 °C Yes 2 mL HPLC-UV

LN19 yes YES / not controlled Yes 400 ml 70°C Yes between 4 and 14 ml LC-MS/MS
LN20 yes YES 71 calibrated thermometer Yes 463 ml 68.1 - 70.0 No LC-MS/MS
LN21 other, please Migration step is accredited YES 73 C calibrated thermometer No 400 ml Yes average of 5 mL HPLC-UV
specify below together with the analite
determination; we do not have
accreditation for the migration
step by it self.

LN22
LN23 yes accreditation of procedure is YES 73°C calibrated thermometer Yes 460 ml Yes HPLC-DAD
part of the method

LN24 no YES 72°C calibrated datalogger No 400 ml Excel file sent by e-mail. Yes 1 ml (1st migration test), LC-MS/MS
0 ml (2nd and 3rd
migration test)

LN25 yes European Standard CEN-EN YES 74 ºC calibrated datalogger No 450 ml 70 ºC (with an tolerance Yes Looses in MIG1=5 mL, LC-MS/MS
13130-1 and Regulation (EU) No range of 2 ºC) MIG2=5 mL and MIG3=10
10/2011 mL
LN26 no YES 75 °C calibrated datalogger No 420 ml Yes No losses LC-MS/MS
LN27 yes YES 70 °C calibrated datalogger Yes 400 ml 68-71 °C Yes 2.0-2.8 mL LC-MS/MS

LO30 yes YES in an oven at 75 °C calibrated datalogger No 430 ml Around 70.5°C (see the No HPLC-DAD
datalogger)

LO31 yes YES 75 °C calibrated thermometer Yes 420 ml 70 °C No LC-MS/MS

LO32 yes we are flexibly accredited in the YES 71 °C calibrated thermometer Yes mug 1/2/3:460 ml, separate Excelsheet (Mail) Yes 10 LC-MS/MS
field of migration studies mug 4: 450 ml

51
LC Code Accreditation Please specify Did you pre-heat Temperature of How did you control the Did you Volume of the food Temperature of the food Did you If yes, please report the Analytical
for the the simulant the food simulant temperature of the food preheat the simulant used for the simulant during the measure the volume of the losses in techniquecs
migration before filling the before filling of simulant during the mugs before migration experiments migration experiment (in oC) food simulant ml for melamine
procedure? artide? the test items migration experiments migration? losses
LO33 yes YES 70 °C calibrated datalogger No 400 ml 68,0 - 69,9 °C No HPLC-DAD

LO34 other, please The migration procedure is part YES 75 °C calibrated datalogger Yes 440 ml No LC-MS/MS
specify of the accredited methods for
below melamine and formaldehyde.

LO35 yes YES 70 °C calibrated datalogger No for each experiment the temperature is No HPLC-DAD
450 ml controlled in a preheated
beaker

LO36 yes YES 70 °C calibrated thermometer No 400 ml please see excelsheet by No HPLC-DAD
separate mail

LO37 yes YES 73 °C calibrated thermometer No 455 ml 70°C No LC-MS/MS

LO38 no YES 70 °C calibrated thermometer No 450 ml 70°C No LC-MS/MS

LO39 yes YES 70 °C calibrated datalogger No 400 ml Please see attachment No HPLC-DAD

LO40 no YES 70 °C calibrated thermometer Yes 460 ml 69.4°C No other, please

specify below
LO43 no YES 70 °C calibrated datalogger No 470 ml No HPLC-UV

LO44 other, please accreditating since october 2023 YES 70 °C calibrated datalogger No 410 ml 70°C No HPLC-DAD
specify below
LO45 yes YES 72 ºC calibrated thermometer Yes 450 ml 70 ºC No LC-MS/MS

LO46 yes YES 73 ºC calibrated datalogger No 466 ml No other, please

specify below
LO47 yes YES 70 ºC calibrated datalogger No 450 ml Yes 25 ml ca. LC-MS/MS

LO48 yes UNE-EN 13130.1 YES 73-74ºC calibrated datalogger Yes 450 ml MIG 1 (Media: 70.1ºC) // MIG Yes In case of loss of LC-MS/MS
2 (Media: 69.8ºC) // MIG 3 simulant, it is replaced up
(Media: 70.4ºC) to the original starting
volume.

52
LC Code LOQ for melamine Sample preparation for Analytical techniques LOQ for fo Time (in hours/days) between the surface to volume ratio applied to the test result Any problem encountered?
in food simulant B? formaldehyde? for formaldehyde rmaldehyde in food migration experiments (MIG1, MIG2
simulant B' and MIG3)

1 19 20 21 22 23 24 25
LN01 0.1 mg/kg acetyl acetone (AA) Spectrophotometry 2.5 mg/kg 1 day (same starting time) concentration per area calculated using c * 0.41 l Measurement uncertainty could only be entered for the first migration
/ 2.78 dm² and then 6 dm² / 1 kg applied acc. each, but unfortunately only as decimal, not in percent. Therefore, it does
article 17(2) not apply to second and third migrations. The field length for Q2 and Q4
was way too short to be "as detailed as possible", as was requested in the
instructions.
LN02 0.001 mg/kg acetyl acetone (AA) HPLC-UV 1 mg/kg MIG 1 to MIG 2 : 10min ; MIG 2 to MIG Yes, Volume : 0.42L ; surface 2.78 dm² On of the 4 cups cracked during experiments. The results of the 3 other
3 : 20 min cups was taken into account
LN03 1.0 mg/kg chromotropic acid Spectrophotometry 1.5 mg/kg 0.25 h (15 min) after compleating of 2.58 : 0.4 = 6.45 No
the previous migration

LN04 - chromotropic acid Spectrophotometry 0,92 mg/L All experiment were made in 2 working No ratio applied. No.
days.
LN05 0.25 mg/Kg acetyl acetone (AA) Spectrophotometry 1.5 mg/Kg 1hr between MIG1/MIG2 and 18h not applicable No
between MIG2/MIG3
LN06 0.25 mg/Kg chromotropic acid Spectrophotometry 1.5 mg/Kg 1hr between MIG1/MIG2 and 18h not applicable No
between MIG2/MIG3
LN07 0.00007 mg/kg acetyl acetone (AA) Spectrophotometry 0.1 mg/kg 1 hour 3.07 dm2 : 0.47 l

LN08 0.25 mg/kg acetyl acetone (AA) LC-MS/MS 1,5 mg/kg 0.1 hour 6 Not enough space for commenting on question 1 and 3: "Although no
common agreement has been reached on harmonised procedure for
checking stability we are reporting according to: Each migration result has
uncertainty based on our analytical method validation and a coverage
factor of 2. Non compliant if m1<m2 or m2<m3 or m1<m3 (result >=
LN09 0.25 mg/kg acetyl acetone (AA) LC-MS/MS 1.5 mg/kg 1 6 no

LN10 0,5 mg/kg acetyl acetone (AA) Spectrophotometry 3 mg/kg mig1 -> 18 h -> mig2 -> 2 h -> mig3 6 dm2/l no
LN11 0.1 mg/kg acetyl acetone (AA) Spectrophotometry 1 mg/kg 22 h (MIG1 - MIG2), 0.5 h (MIG2 - 2.96 dm² / 0.47 L datalogger failure (migration 1 and 2) + evaporation in the mug used for
MIG3) the temperature monitoring (temperature underestimated, migration 3)

LN12 0,5 mg/L 2,4- HPLC-UV 1 mg/L 4 hours between mig 1 and mig 2 and real surface volume ratio no
dinitrophenylhydrazine 24h between mig 2 and mig 3
LN13 5 µg/L acetyl acetone (AA) Spectrophotometry 0.5 mg/L MIG1 -> MIG2: 38 min / MIG2 -> MIG3: Filling volume and calculated surface of mugs Dispatch of ILC test items was delayed over the weekend.
37 min (2.62 dm^2) were applied to the raw migration
results. Results were converted to kg using a
surface to volume ratio of 6 dm^2/kg.

LN14 0.25 mg/L acetyl acetone (AA) Spectrophotometry 1,5 mg/L 1 day (MIG1, MIG2 and MIG3 were 6 dm2/kg No
performed in 3 consecutive days)
LN15 1,86mg/kg acetyl acetone (AA) Spectrophotometry 0,33mg/kg 2 hours 1:2 no

LN16 0.25mg/kg other, please specify Spectrophotometry 0.3 mg/kg 20 mins Yes No
below
LN17 0.25 mg/Kg chromotropic acid Spectrophotometry 2 mg/Kg Tests are carried out in the same time - -

LN20 1.0 µg/L acetyl acetone (AA) HPLC-UV 0.03 mg/L 0.5 hours 6:1 No

53
LC Code LOQ for melamine Sample preparation for Analytical LOQ for fo Time (in hours/days) between the surface to volume ratio applied to the test result Any problem encountered?
in food simulant formaldehyde? techniques for rmaldehyde in migration experiments (MIG1, MIG2
B? formaldehyde food simulant B' and MIG3)

1 19 20 21 22 23 24 25
LN18 1,6 mg/kg acetyl acetone (AA) Spectrophotometry 1.5 mg/kg 24 hours 6 dm2/kg None

LN19 0.23 mg/kg other, please specify Spectrophotometry 2 mg/kg 1 day at each time 0.001 none
below
LN20 1.0 µg/L acetyl acetone (AA) HPLC-UV 0.03 mg/L 0.5 hours 6:1 No
LN21 0.23 mg/kg acetyl acetone (AA) Spectrophotometry 1.75 mg/kg 0.25 hours Real ratio A/V Time to reach the test temperature due to the type of article and the
volume of the test. The mugs seemed to be made with isolated material
turning the transference of the temperature thru the mugs wall very
difficult. The control of the 2nd test temperature was facilitated because
the mugs were already warm from the 1st test.

LN22
LN23 0.6 mg/kg acetyl acetone (AA) Spectrophotometry 3.00 mg/kg MIG1 - MIG2 (15 min); MIG2-MIG3 (19 2.79 square dm / 460 ml no
min), total time between MIG1-MIG3
(2 hours and 34 min)
LN24 0.25 mg/kg chromotropic acid Spectrophotometry 3 mg/kg 3 minutes Surface to volume ratio 6 dm2 / 1000 ml was no
applied to the test results (because volume at
migration test was 400ml, surface of the sample
was 2.43dm2).

LN25 0.5 mg/kg chromotropic acid Spectrophotometry 1.4 mg/kg 24 hours between MIG1 and MIG3 S/V (dm2/kg)=6 Accidental loss of food simulant during the filling of MUG3 in MIG3.
(Last migration process).

LN26 0,001 mg/kg acetyl acetone (AA) HPLC-UV 1 mg/kg Between MIG 1 and 2: 13 min. Yes. Surface 2,78 dm2 Volume 0,42 l One of the cups cracked during migrations.
Between MIG 2 and 3: 18 h.
LN27 0.1 mg/L acetyl acetone (AA) Spectrophotometry 0.1 mg/L <0.25 h 2.336 dm2/400 mL We suspect hexamethylenetetramine (HMTA) and 1,4-butanediol formal –
if present – to be decomposed and forming formaldehyde during
migration testing (acidic, 70 °C). An issue to be investigated in the future.

LO30 0,5 mg/kg 2,4- HPLC/DAD 3 mg/kg 17h between MIG1&2 (consecutively No because could be used by children < 3 yo. The No
dinitrophenylhydrazine performed) and MIG3. See datalogger Surface in contact is 2.94 dm² and the filling
volume 430 mL
LO31 0,25 mg/kg acetyl acetone (AA) Spectrophotometry 0,13 mg/kg MIG1 Day 1, MIG 2 and MIG 3 day 2, 6 mg/dm² (results are normalised) MUG 4 was broken, MUG 5 was also analyzed, results are much higher,
intervall 1 h see attached file via mail.
LO32 0,03 mg/l acetyl acetone (AA) Spectrophotometry 0,9 µg/25ml all experiments in one day, ca. 45 min mug 1-3: 6 dm²/l, mug 4: 6,2 dm²/l one of the cups had significantly lower migration values for melamine and
between tests formaldehyde and was therefore not included in the data submission.
LO33 1,22 mg/kg 2,4- HPLC/DAD 0,70 mg/kg MIG1 to MIG2: 5 min; MIG2 to MIG3: 6 volume: 400 mL; contact surface: 2,92 dm² / and no
dinitrophenylhydrazine min (time between the migration tests) surface to volume ratio 6 dm² per kg of food

LO34 0.03 mg/kg 2,4- HPLC/DAD 1 mg/kg MIG1, MIG2 and MIG3 were performed 6.0 dm²/L During migration a little piece of plastic broke from the inner bottom of
dinitrophenylhydrazine in direct succession with a few minutes one of the 4 mugs. Consequently, this mug was not considered for the
in between. reported migration values.
LO35 0,14 mg/kg acetyl acetone (AA) Spectrophotometry 0,6 mg/kg only few minutes, all migrations within 6.47 no
one day
LO36 0.25 mg/kg acetyl acetone (AA) Spectrophotometry 0.9 mg/kg time between the migration 6 dm2/kg no
experiments under 5 minutes

54
LC Code LOQ for melamine Sample preparation for Analytical LOQ for fo Time (in hours/days) between the surface to volume ratio applied to the test result Any problem encountered?
in food simulant formaldehyde? techniques for rmaldehyde in migration experiments (MIG1, MIG2
B? formaldehyde food simulant B' and MIG3)

1 19 20 21 22 23 24 25
LO37 0.25 mg/kg chromotropic acid Spectrophotometry 1.5 mg/kg the three mugs were analyzed 0.6 It's not clear to which values apply the uncertainty of the method in the 3
simultaneously tests. It was decided to apply it to the first test for each mug

LO38 0.3 mg/Kg chromotropic acid Spectrophotometry 2.0 mg/Kg 8 days for Formaldehyde; 16 days for 0,6
Melamine
LO39 0.1 mg/Kg 2,4- HPLC/DAD 2 mg/Kg 1 day 3.12 dm2 no
dinitrophenylhydrazine

LO40 0 chromotropic acid Spectrophotometry 1.50 mg/kg MIG1-MIG2 30 minutes; MIG2-MIG3 YES NO
two days
LO43 0.5 mg/Kg chromotropic acid Spectrophotometry 3 mg/Kg 5 minutes 6 dm2/L No problems encountered

LO44 0,1 mg/kg 2,4- HPLC/DAD 1,5 mg/kg 10 minutes not applied no
dinitrophenylhydrazine
LO45 0.2 mg/Kg chromotropic acid Spectrophotometry 3 mg/Kg 0 hours, in successive incubations, one 6 (dm2/Kg) /6.3 (dm2/Kg) = 0.95 NO
after the other on the same day.
LO46 0,0 chromotropic acid Spectrophotometry 3 mg/kg 3 days 6 dm2/kg No

LO47 0.05 mg/kg 2,4- HPLC-UV . 2 days 0.66 Some difficulties for maintaining mug temperature
dinitrophenylhydrazine
LO48 LOQ = 0.1 mg/Kg chromotropic acid Spectrophotometry LOQ = 3 mg/Kg MIG 1 (25/07/23, 13:30-15:30) // MIG 6.0 dm2/Kg (according Reg 10/2011, article 17, No
2 (26/07/23, 9:00-11:00) // MIG 3 articles less than 500 millilitres
(26/07/23, 12:40-14:40)

55
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