Testing of food contact materials

Viviana Golja, MSc.

 Overview

Testing of:
– Plastics
– Ceramics
– Metalls and alloys
– Paper & board
– Coatings
Conclusion
 FCMs: Regulation 1935/2004
ANNEX I:
1. Active and intelligent materials and articles
2. Adhesives
3. Ceramics
4. Cork
5. Rubbers
6. Glass
7. Ion-exchange resins
8. Metals and alloys
9. Paper and board
10. Plastics
11. Printing inks
12. Regenerated cellulose
13. Silicones
14. Textiles
15. Varnishes and coatings
16. Waxes
17. Wood
 All FCMs:
SAMPLING:
• Representative
• careful handling and preserving the samples
(segregation, protection from light, temperature, moisture,
volatiles, test repetition)
Plastics
 Plastics

• Plastics REGULATION (EU) NO 10/2011

– Overall migration
– Specific migration
– Examples
– Prevailing approach
• Guidance documents
 Plastics
General terms
• Overall migration (OM):
• total of substances that can migrate (gravimetric analyses)
• Measure of inertness
• Unit: mg/dm2 (except for FCMs for infants and young children)

• Specific migration (SM):

• quantity of one specific substance that migrates
• Unit: mg/kg
 Plastics
Restrictions & specifications

• Overall migration limit (OML)

• Specific migration limit (SML)
• Total specific migration limit (SML(T) )
• Residual content per food contact surface area
(QMA)
• Concentration in final product
• Specification
 Plastics
Examples:
OML is 10 mg/dm2 (before also 60 mg/kg)
SML for formaldehyde is 15 mg/kg
QMA for vinyltriethoxysilane: 0,05 mg/dm2
Concentration in final product: phthalic acid, benzyl butyl ester – if
technical support agent in concentrations up to 0,1 % in the final
product
Specification: waxes...high viscosity: …Content of mineral
hydrocarbons with carbon number less than 25, not more than 5 %
(w/w).
 Plastics
Separate sets of testing conditions for overall migration
and specific migration

Revised exposure time and temperature parameters for

specific migration testing
New simulant = Tenax (for dry foods)

Screening tests (extraction, calculation, modelling) and

verification test (migration testing)
 Plastics

Specific migration testing: plastics already in contact with

food:
• Sample preparation
• Analysis of migrated substances
• Special cases (e.g. phthalates)
 Plastics: compliance testing
• PIM Annex V

– Testing for specific migration of materials and

articles already in contact with food
– Testing for specific migration of materials and
articles not yet in contact with food
– Testing for overall migration
– Correction factors applied when comparing
migration test results with migration limits
 Specific migration testing:
plastics not yet in contact with food
Verification method:
Determination of specific migration (SM)
mimicking real migration into food
• Use of simulants, t, T, S / V and worst case conditions

Sreening methods – for SM testing and OM testing

 Specific migration testing:
plastics not yet in contact with food
• Contamination before contact?
• Sample preparation (instruction for use, DoC?,
representative specimen? Only parts intended to come
into contact)
• Repeated use articles (3 X, substances non detectable
and not listed – 1X)
• Analysis of migrated substances in simulant

• Conventional migration tests

 Specific migration testing:
plastics not yet in contact with food
 Specific migration testing:
plastics not yet in contact with food
contact with all types of foods:

A : Ethanol 10 %
B: Acetic acid 3 %
D2: Vegetable oil

contact with only dry foods:

E: Tenax

If intended only for specific types of foods:

Table II in Annex III
 Specific migration testing:
plastics not yet in contact with food
 Specific migration testing:
plastics not yet in contact with food
 Specific migration testing:
plastics not yet in contact with food
Specific conditions for contact times above 30 days at
room T and below:
• accelerated test at elevated temperature:
max. 10 days at 60 °C
• t and T conditions based on the following formula.
• t2 = t1 * Exp ((-Ea/R) * (1/T1-1/T2))

• Calculator!
 Specific migration testing:
plastics not yet in contact with food
Specific conditions for contact times above 30 days
at room T and below:
10 days at 20 °C =all storage times at frozen
condition
10 days at 40 °C = all storage times at refrigerated
and frozen conditions including heating up to 70
°C for up to 2 hours, or heating up to 100 °C for
up to 15 minutes
 Specific migration testing:
plastics not yet in contact with food
Specific conditions for contact times above 30 days at room T
and below:
10 days at 50 °C = all storage time at refrigerated and frozen
conditions including heating up to 70 °C for up to 2 hours, or
heating up to 100 °C for up to 15 minutes and storage times of
up to 6 months at room temperature
10 days at 60 °C = long term storage above 6 months at room
temperature and below including heating up to 70 °C for up to 2
hours, or heating up to 100 °C for up to 15 minutes.
 Specific migration testing:
plastics not yet in contact with food

• Specific conditions for contact times above 30

days at room T and below:
• storage at room temperature = 10 days at 40 °C if
there is scientific evidence that migration of the
respective substance in the polymer has reached
equilibration under this test condition.
 Specific migration testing:
plastics not yet in contact with food
Specific conditions for combinations of contact
times and temperature:
- different combinations of contact time and
temperature the testing = test conditions which are
recognised to be the most severe
- if successively subject to a combination of two or
more times and temperatures = successively to all
the applicable worst foreseeable conditions using
the same portion of food simulant.
 Specific migration testing:
plastics not yet in contact with food

• Repeated use articles

• • 3 X - third test result for compliance
• • First test when proof of no increase and
compliant
• • First test when SML = ND and for non listed
substances used behind FB
 Specific migration testing:
plastics not yet in contact with food

Analysis of migrated substances

 Specific migration testing:
plastics not yet in contact with food

• Residual content per surface area QMA

• For substances unstable in food simulant or

food or for which no adequate analytical
method available = residual content per 6 dm2
 Specific migration testing:
plastics not yet in contact with food

SCREENING

• Replacing specific migration by overall migration

• (only for non-volatile substannces)
• Residual content (calculation of migration
potential)
• Migration modelling
• Food simulant substitutes
 Specific migration testing:
plastics not yet in contact with food

Standardised test conditions:

• 7 standard testing conditions
• 2 alternative test conditions (high
temperature)
 Overall migration testing

•worst foreseeable conditions of use in

which changes do not take place
 Overall migration testing

all type of foods distilled water or A + B + D2

all types of food except for distilled water or A + D2
acidic foods
all aqueous + alcoholic foods D1
+ milk products
all aqueous, acidic and B + D1
alcoholic foods and milk
products
all aqueous foods and C
alcoholic foods up to an
alcohol content of 20 %
all aqueous + acidic foods + C+B
alcoholic foods up to an
alcohol content of 20 %
Overall migration testing
Overall migration testing
 Overall migration testing

• Substitute test for OM7 with food simulant

D2
• If technically not feasible to perform OM7
with food simulant D2 OM 8 or OM9 can be
used with a new test sample.
Overall migration testing
 Overall migration testing

• Repeated use articles

contact – 3 X
• Compliance testing= level of the migration
found in the third test (if level is not increased
and not exceeded in first test)
 Overall migration testing

SCREENING:
More severe than the verification method:
• Residual content (Calculation based on the
residual content of migratable substances
determined in a complete extraction of the
material or article)
• Use of food simulant substitutes
 Overall migration testing

• Correction of migration into food simulant D2

• For some food categories migration test result
into food simulant D2 shall be divided by
written figure before comparing with the
migration limit 10 mg/dm2
 Methods for OM and SM testing

total immers. migration cell article filling

• Specific migration testing – more important then

overall migration testing
 Examples

• Yogurt cup
– Food simulants – B (if pH<4,5) and D1
– OM conditions – OM1 (10 d at 40ºC)
– SM conditions - 10 days at 40 °C (covers all storage times at
refrigerated and frozen conditions including heating up to 70 °C
for up to 2 hours, or heating up to 100 °C for up to 15 minutes).
– Testing cups by article filling method or plastic sheets by total
immersion method; because V cup<0,5L, results of specific
migration should use the relation of 6dm2/1kg of food.
 Examples
• PET bottle for juice (clear drink):
– Food simulants – B (if pH<4,5) and C
– OM conditions – OM2 (10 d at 40 °C)
– SM conditions - 10 days at 60 °C (shall cover long term
storage above 6 months at room temperature and below
including heating up to 70 °C for up to 2 hours, or heating
up to 100 °C for up to 15 minutes)
– Testing bottles by article filling method; if V bottle> 0,5L
and <10L, results of specific migration shall be expressed in
mg/kg applying the real surface to volume ratio in actual
or foreseen use, if V bottle <0,5L, results of specific
migration should use the relation of 6dm2/1kg of food.
 Examples
• Plastic plate
– Food simulants – Materials and articles intended
for contact with all types of food shall be tested
with food simulant A, B and D2.
– OM conditions – OM3 (2 hours at 70 °C)
– SM conditions - Testing for 2 hours at 70 °C.
– Testing plates by article filling method or by total
immersion method; if V plate<0,5L, results of
specific migration should use the relation of
6dm2/1kg of food.
 Prevailing approach

• OM testing
• Results of verification prevail over results of
screening

• SM testing
• Results in food prevail over results in
simulants
• Results in simulants prevail results over
screening
 Guidance documents

Google EURL FCM

http://ihcp.jrc.ec.europa.eu/our_labs/eurl_food_c_m/guidance-documents
 Ceramics

• Specific migration of Pb and Cd:

– 4 % (v/v) acetic acid, in a freshly prepared
aqueous solution
Test conditions
• 22 ± 2 °C for a duration of 24 ± 0,5 hours.
Metals and alloys
Metals &alloys: CoE Practical Guide

Art. 3 Regulation 1935/2004

• Release testing – new approach:

– new simulants
– envelope volume
– SRLs
Metals &alloys: CoE Practical Guide
• Release testing into foodstuffs
• Testing of packaged food
• Utensils
Metals &alloys: CoE Practical Guide
Transitional SRLs

0,2
1
0,1

0,6
0,7

0,05
Practical Guide

Transitional SRLs
0,01

0,05
0,02
0,04

0,015
0,0005
Metals &alloys: CoE Practical Guide
Envelope volume = X × Y × Z (in cm3)

RW (kg) = Envelope volume (cm3) /1000

Metals &alloys: CoE Practical Guide

Released mass (M) = V × C

V: volume of simulant used

C: Concentration of the element to be
examined in the simulant

Determination of the specific release:

As a general rule: SR = M/RW

Paper and board
 Paper and board
• Standards: Paper and board intended to come into
contact with foodstuffs
• Cold water extract EN 645
• Hot water extract EN 647
• Conditions for migration testing with MPPO EN
14338
+ determination of specific substance
or extraction of the material + determination
• Preparation of an organic solvent extract EN 15519
 Paper and board
• Hydrocarbons from mineral oils (Mineral oil
saturated hydrocarbons (MOSH) and mineral
oil aromatic hydrocarbons (MOAH) and
plastics (Polyolefin oligomeric saturated
hydrocarbons (POSH) & Poly alpha Olefine
(PAO)) in packaging materials and dry
foodstuffs :
• solid phase extraction + GC-FID
 Paper and board
• Organoleptics testing:
CEN/TR 15645-1:2008
CEN/TR 15645-2:2008
CEN/TR 15645-3:2008
EN 1230-1:2010
EN 1230-2:2010
CEN/TR 15645-2:2008/AC:2009
CEN/TR 15645-3:2008/AC:2009
Coatings
 Coatings
Art. 3 Regulation 1935/2004

Test conditions according to JRC Guidelines

(volontary)
CEN/TS 14235: Materials and articles in contact
with foodstuffs - Polymeric coatings on metal
substrates - Guide to the selection of conditions
and test methods for overall migration
 Conclusion

Testing of FCMs is
complex and demanding task