Selecting Food Simulants under EU Regulation Ten Eleven

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A laboratory test report declaring overall migration below 10 milligrams per square decimeter in 10 percent ethanol arrived with a consignee shipment of high-density polyethylene dispensing spouts intended for extra virgin olive oil. The laboratory test failed immediately. High-density polyethylene exposed to pure vegetable oils yields substantial lipophilic interaction, yet the importer accepted documentation showing testing performed solely with aqueous simulants.

Testing food contact plastics requires selecting exposure media strictly aligned with the intended edible contact substance, codified under Annex III of Commission Regulation (EU) No 10/2011.

Regulation (EU) No 10/2011 governs plastic materials and articles placed on the European Union market. Annex III assigns specific food simulants to replicate extraction properties across distinct chemical categories: hydrophilic, acidic, alcoholic, lipophilic, and dry matrices. Simulants represent conservative extraction baselines.

Overall migration limits verify material inertness, capped at 10 milligrams of total non-volatile substances per square decimeter of plastic contact area (mg/dm²), or 60 milligrams per kilogram of food simulant (mg/kg) for infant containers and specific packaging formats.

An overall migration limit of 10 milligrams per square decimeter applies to all liquid simulants during contact testing for ten days at 40 degrees Celsius.

Simulant Allocations for General Food Contact

Annex III of Regulation (EU) No 10/2011 links chemical properties of packed comestibles directly to designated liquid and solid test media. Testing general or non-specific food contact requires demonstrating compliance across multiple exposure chemistries.

• Simulant A represents clear aqueous foodstuffs with neutral or buffered chemical behavior at pH values exceeding 4.5, formulated as 10 percent ethanol by volume in distilled water.
• Simulant B addresses acidic comestibles displaying pH values at or below 4.5, prepared as 3 percent acetic acid by weight in aqueous solution. Acetic acid attacks zinc stearate stabilizers.
• Simulant C simulates alcoholic matrices containing up to 20 percent ethanol, formulated as 20 percent ethanol by volume, while covering products containing relevant organic lipophilic fractions like specific clear syrups.
• Simulant D1 targets alcoholic media exceeding 20 percent ethanol alongside oil-in-water emulsions, formulated as 50 percent ethanol by volume.
• Simulant D2 represents vegetable oils containing free fatty acid triglycerides, utilizing refined olive oil, sunflower oil, or standardized synthetic triglyceride mixtures.
• Simulant E captures migration into dry, non-fatty comestibles, consisting of synthetic poly(2,6-diphenyl-p-phenylene oxide) with particle dimensions between 60 and 80 mesh. Tenax acts as a vapor trap.

Table Two Assignments across Comestible Categories

Annex III lists specific food matrices by numeric reference, establishing binding test media for each item. When an article contacts a defined foodstuff, testing focuses exclusively on the simulants specified in Table 2 rather than the universal battery.

Articles intended for universal contact with all food categories undergo verification against Simulants B, D2, and E. Simulant A substitutes for Simulant D2 only when the material exhibits physical degradation in hot vegetable oil and technical validation justifies the exclusion. If an article holds only acidic beverages, testing with Simulant B suffices. If a closure seals bottles containing dry flour, testing with Simulant E provides the complete regulatory defense.

Purchasers insert the European standard EN 1186 verification clause into resin supply agreements, obliging suppliers to submit full Annex III extraction data before loading bulk containers.

Bath

Laboratory chemists evaluate plastic articles using sealed stainless steel migration cells, glass exposure jars, or direct pouch filling. Contact methods dictate analytical precision. Total immersion exposes exterior container walls, cut edges, and interior surfaces simultaneously, skewing migration calculations unless outer coatings remain completely inert.

Single-side contact cells restrict simulant exposure to the food-facing polymer boundary, mirroring real-world container mechanics.

Contact Cells and Immersion Procedures

Standard EN 1186 dictates specimen geometry and liquid volumes for overall migration determinations. Liquid simulants require a standardized surface-to-volume ratio, conventionally fixed at 6 square decimeters of contact area per kilogram of food simulant (6 dm²/kg) unless packaging geometry enforces an alternative reality. Specimen edges cut from thermoformed trays expose core layers of multi-layer coextrusions.

Raw ethylene vinyl alcohol (EVOH) barrier cores dissolve when exposed directly to aqueous Simulant B along exposed slice lines. Single-side cells prevent edge-wicking artifacts by clamping an O-ring directly onto the interior functional face.

Article 15 of Regulation 10/2011 invalidates declarations of compliance whenever supporting analytical records lack traceable resin batch identifiers.

Standard Testing Conditions across Temperature Bands

Annex V Table 3 defines standardized contact exposures ranging from OM1 to OM7. These accelerated parameters simulate real-world thermal histories encountered throughout storage, distribution, and culinary preparation.

Operating migration testing under OM2 represents the baseline benchmark for ambient shelf-stable packaging. Ten days at 40 degrees Celsius accelerates six months of room-temperature interaction. Higher thermal excursions demand elevated test regimes.

A polypropylene microwave tray designed for reheating chili requires testing under OM3 (2 hours at 70 degrees Celsius) or OM5 (2 hours at 100 degrees Celsius) depending on target fat temperatures. Migration increases at higher temperatures. Solvent temperature governs laboratory migration rates more aggressively than contact duration.

Fat

Vegetable oil represents the regulatory benchmark for lipophilic comestibles under Simulant D2. Olive oil contains triglycerides that extract plasticizers, slip additives, and antioxidant degradation products far more aggressively than aqueous media. Analytical extraction using olive oil creates practical laboratory bottlenecks.

Gravimetric overall migration measurement demands quantifying milligrams of extracted polymer additives against hundreds of grams of non-volatile triglyceride oil. Chemists quantify migration gravimetrically only after saponifying, methylating, and measuring absorbed oil inside the plastic via gas chromatography with flame ionization detection (GC-FID).

Polymer swelling in volatile organic solvents artificially accelerates additive extraction beyond true contact equilibrium.

Does Simulant D2 Trigger Matrix Swelling?

Polyolefin networks absorb low-molecular-weight triglycerides during prolonged high-temperature exposure. Vegetable oil dissolves low-molecular oligomers. When olive oil penetrates polypropylene or low-density polyethylene at 40 degrees Celsius or 100 degrees Celsius, triglycerides plasticize amorphous regions.

This solvent uptake increases free volume between polymer chains. Additives diffuse outward along accelerated mass-transfer paths that never occur during cold milk or water contact. Standard EN 1186-2 quantifies absorbed oil by extracting fatty acid methyl esters from specimen plaques post-exposure.

The baseline analytical uncertainty sits at plus or minus 2.0 mg/dm² under EN 1186-2; oil retention within the polymer matrix shifts this margin, invalidating results when the polymer absorbs more than 1 percent oil by mass.

Because Simulant D2 presents severe analytical hurdles, Annex III Section 4 permits substitute simulants when testing with vegetable oil becomes technically infeasible. Isooctane, 95 percent ethanol, and modified polyphenylene oxide function as recognized replacement media. Testing with isooctane for 2 days at 20 degrees Celsius replicates 10 days of olive oil contact at 40 degrees Celsius for non-polar polyolefins.

Isooctane evaporates cleanly, enabling direct gravimetric weighing of the migration residue in a tared aluminum dish.

Reduction Factors and Extraction Artifacts

Regulation 10/2011 permits mathematical divisors to reflect actual consumer exposure when articles touch lipophilic substances. Fatty Food Reduction Factors (FRF) divide measured Simulant D2 migration values by numbers between 1 and 5. The factor accounts for the true fat content of the foodstuff.

Whole milk contains approximately 3.5 to 4 percent fat, corresponding to an assigned FRF divisor of 5 under Table 2 Reference 07.01. Chocolate spread containing 30 percent fat earns an FRF divisor of 3 under Reference 05.01.

Application of the reduction factor follows strict statutory boundaries under Article 11. The FRF applies only to Simulant D2 migration values. The reduction factor cannot be applied to substitute solvents like 95 percent ethanol or isooctane unless specific correlation data validates the calculation.

The factor cannot reduce overall migration values below the statutory limit; it applies strictly to specific migration limits (SML) of listed additives.

Assume a food contact container constructed from polypropylene with a surface area of 2.0 square decimeters holds 300 grams (0.300 kg) of hazelnut-chocolate paste containing 35 percent fat. The surface-to-volume ratio measures 2.0 dm² divided by 0.300 kg, yielding 6.67 dm²/kg. The resin formulation includes octadecyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate (CAS 2082-79-3), an antioxidant governed by an SML of 6.0 mg/kg under Annex I. Laboratory testing in olive oil (Simulant D2) under condition OM2 (10 days at 40 °C) returns an uncorrected additive migration of 15.0 mg/kg.

The test report appears non-compliant. Table 2 Reference 05.01 assigns an FRF of 3 to chocolate paste with this fat profile. Applying the statutory divisor yields a corrected migration value of 15.0 mg/kg divided by 3, resulting in 5.0 mg/kg.

The container complies with the specific migration limit. Stress the core assumption: if the same packaging holds pure roasted peanut butter containing 55 percent fat, the assigned reference shifts to Reference 05.02, lowering the FRF divisor to 1. The corrected migration remains 15.0 mg/kg.

The container fails compliance immediately.

Common analytical pitfalls distort fatty simulant assessments during commercial qualification:

• Unqualified Solvent Substitution where laboratories run 95 percent ethanol instead of vegetable oil without recording the technical impossibility of testing in Simulant D2, invalidating the declaration under regulatory scrutiny.
• Illegal Divisor Application involving chemists applying the FRF divisor directly to isooctane gravimetric totals, masking structural additive bleed through unjustified mathematical reductions.
• Additive Saponification Losses occurring when ester-based slip agents like erucamide break down during basic saponification of absorbed olive oil, understating specific migration values by 40 percent.
• Matrix Plasticization Distortion whereby volatile solvents dissolve low-molecular polyethylene oligomers at ambient temperatures, producing artificial non-volatile residues not present in vegetable oil contact. The solvent swells polyolefin chains.

Selecting an unlisted substitute solvent invalidates the conformity dossier, triggering administrative product withdrawals and customs impoundment at the port of entry.

Stress

Repeated mechanical deformation and elevated thermal history alter polymer morphology between manufacturing and final kitchen contact. Standard laboratory tests on pristine, unprinted test plaques fail to predict additive migration from finished, mechanically formed articles. Stress cracking, thermal oxidation, and post-crystallization shift chemical diffusion rates across polyolefin and polyester matrices.

Which Contact Regimes Demand Simulant E?

Modified polyphenylene oxide serves as the prescribed medium for dry foodstuffs under Annex III Table 1. Dry contact relies on vapor-phase diffusion and direct surface abrasion rather than liquid dissolution. Sugar, dry grain flour, pasta, and infant milk powders contact Simulant E during compliance qualification.

In analytical instrumentation, Tenax captures volatile organic compounds with exceptional thermal stability. Identical macro-porous polyphenylene oxide polymer sorbents capture trace volatile gases on high-altitude geological sampling probes and spacecraft atmospheric air reclamation units without undergoing chemical degradation. In food contact laboratories, this high-surface-area solid adsorbent mimics the high affinity dry cereal powders exhibit for low-molecular polymer additives.

Testing with Simulant E operates under EN 14338. Tenax coats test specimens at a concentration of 4 grams per square decimeter of plastic surface. Following thermal exposure (such as 10 days at 40 degrees Celsius for ambient dry goods storage), the chemist pours off the loose Tenax powder and extracts sorbed migrants using diethyl ether or acetone.

The solvent evaporates prior to analysis via gas chromatography coupled with mass spectrometry (GC-MS). High-density polyethylene caps intended for powdered infant formula require testing with Simulant E. If an importer presents migration data derived solely from 10 percent ethanol (Simulant A) for dry infant cereal packaging, border control chemists reject the dossier.

Repeated Exposure and Non-Intentionally Added Substances

Multi-use kitchenware requires three consecutive migration cycles using fresh test aliquots for each exposure. Blenders, coffee machine tubing, reusable water bottles, and conveyor belts undergo three separate extractions under Article 21. Compliance evaluates migration measured strictly during the third test cycle.

Third extraction values determine compliance.

1. Initial Extraction Phase exposes the virgin plastic article to the selected simulant for the defined time and temperature period, capturing initial bloom of manufacturing lubricants, surface static inhibitors, and dusting agents.
2. Intermediate Purge Cycle empties the initial simulant volume and exposes the article to a second fresh simulant charge, measuring intermediate release rates while documenting whether additive extraction attenuates or accelerates.
3. Definitive Compliance Assessment executes the third consecutive exposure with a new simulant volume, requiring that the measured migration remains below the specific migration limit and confirms that migration levels decrease across successive cycles.

An article showing an increasing migration trend across cycles one, two, and three fails compliance regardless of whether absolute numbers remain below the numerical SML. Increasing migration signals structural degradation or progressive chemical dissolution of the polymer matrix under simulant attack.

Repeated thermal exposure accelerates the formation of non-intentionally added substances (NIAS). Reaction side-products, polymer breakdown fractions, and additive impurities migrate into food simulants alongside intentionally added stabilizers. Regulation 10/2011 Article 19 mandates risk assessment of these unlisted components.

Non-intentionally added substance identification utilizes gas chromatography and liquid chromatography paired with high-resolution time-of-flight mass spectrometry (GC-Q-TOF and LC-Q-TOF). The analytical baseline shifted upward. Under standard toxicology screening assumptions, any unlisted non-carcinogenic migrant exceeding 10 micrograms per kilogram (10 ppb) requires toxicological characterization.

The literature reports non-intentionally added substance migration screening false-positive rates of 18 percent when using gas chromatography coupled with time-of-flight mass spectrometry on recycled polyolefins. The desk cannot defend that exact 18 percent figure across diverse resin grades. Sourcing managers handle this unquantified margin by demanding liquid chromatography high-resolution mass spectrometry confirmations on every volatile library hit exceeding 10 micrograms per kilogram.

Suppliers defend non-intentionally added substance detections by claiming volatile peaks represent harmless atmospheric background contamination absorbed during warehouse storage.

Claim

A Declaration of Compliance transfers technical liability from resin compounders through converters to retail brand owners. Article 16 of Regulation (EU) No 10/2011 establishes the statutory obligation for all plastic food contact materials placed on the market. The declaration functions as an executive summary of conformity, backed by the detailed supporting documentation file mandated under Annex IV.

Border control authorities detain imported consignments when migration dossiers reference unlisted resin trade designations.

Declaration Scope across Component Chains

Article 16 and Annex IV of Regulation 10/2011 mandate clear documentation of intermediate additives and processing aids. Upstream raw resin certificates prove nothing downstream. Extruders add slip masterbatches, converters apply solvent-based laminating adhesives, and printers apply curable inks.

Each processing step introduces new chemical migrants and alters crystallization behavior. A converter must not copy the polymer producer’s declaration without testing the finished composite.

Annex IV specifies nine mandatory elements for a valid Declaration of Compliance:

The identity and address of the business operator issuing the declaration establishes commercial accountability. The identity of the manufacturer or importer placing the plastic article onto the market confirms jurisdiction. The commercial trade name of the finished material or intermediate article identifies the physical lot.

The confirmation date proves regulatory currency under recent amendments. Confirmation that the plastic material complies with relevant requirements of Regulation 10/2011 and Framework Regulation (EC) No 1935/2004 defends basic legality. Adequate information regarding dual-use additives subject to purity criteria or food additive restrictions prevents cross-regulation violations under Regulation (EC) No 1333/2008.

Specifications on the use of the material, including food categories, contact duration, and temperature ranges, define safe operational envelopes. When migration modeling demonstrates compliance, supporting calculations must accompany the dossier. The functional barrier confirmation documents absence of migration across multi-material multi-layer structures.

Customs Retention and Testing Inconsistencies

European port authorities execute random spot sampling on imported food contact plastics. Customs inspectors verify batch numbers. Discrepancies between the trade name on the shipping manifest and the test report invalidate the entry.

That certificate covers unprinted film only. Importers absorb storage charges and inspection costs while containers sit in quarantine. Demurrage accumulates daily at the terminal.

The shipment stayed on the quay. The buyer pays the warehouse demurrage.

Auditing the underlying laboratory report requires verifying the detection limits achieved during testing. When a supplier’s laboratory report states that specific migration of primary aromatic amines remains not detected, the statement lacks legal weight without stating the analytical limit of detection (LOD). Under Regulation (EU) 2020/1245 amending Regulation 10/2011, primary aromatic amines listed in Annex XVII to REACH carry an individual detection limit of 0.002 milligrams per kilogram (2 ppb).

A laboratory screening report configured with an LOD of 0.01 mg/kg leaves the importer open to enforcement penalties. Regulatory authorities leave open whether chemically recycled post-consumer resins require complete non-intentionally added substance re-characterization for every production lot or periodic verification against initial qualification baselines.