Tests to be Performed Within the Scope of Directive 84/500/EEC

Council Directive 84/500/EEC aims to approximate the laws of the Member States regarding ceramic products intended to come into contact with foodstuffs. The method in this directive allows the determination of the specific migration of lead and/or cadmium. In principle, the determination of the specific migration of lead and/or cadmium is carried out by atomic absorption spectrophotometry.

The basic rules for determining lead and cadmium migration are set out in the annex of the Directive as follows (Annex I):

• Test liquid (simulant): 4 percent (v/v) acetic acid in freshly prepared aqueous solution.
• Test conditions: The test is performed at a temperature of 22°C plus/minus 2°C for 24 hours plus/minus 0,5 hours. If lead migration is to be determined, the sample is covered with a suitable protective device and exposed to the usual lighting conditions in the laboratory. If cadmium or lead and cadmium migration is to be determined, the sample is covered to ensure that the surface to be tested is completely dark.
• Filling: For fillable samples, the substance is filled with a 4 percent (v/v) acetic acid solution to a distance of not more than 1 mm from the overflow point, the distance being measured from the top edge of the sample. Samples with flat or slightly sloping edges should be filled so that the distance between the surface of the liquid and the overflow point is not more than 6 mm when measured along the sloping edge.

For non-fillable samples, the surface of the sample not intended for contact with foodstuffs is first coated with a suitable protective layer capable of withstanding the action of a 4 percent (v/v) acetic acid solution. The sample is then immersed in a container containing a known volume of acetic acid solution so that the surface intended for contact with foodstuffs is completely covered with the test liquid.

• Determination of surface area: The surface area of ​​Category 1 substances is equal to the surface area of ​​the meniscus formed by the free liquid surface obtained by complying with the filling requirements specified above.

Analysis methods for determining lead and cadmium migration are specified as follows (Annex II):

• Purpose and field of application: The method allows the determination of the specific migration of lead and/or cadmium.
• Principle: Determination of the specific migration of lead and/or cadmium is carried out by atomic absorption spectrophotometry.
• Reagents: All reagents should be of analytical grade unless otherwise stated. Where reference to water is made, this always means distilled water or water of equivalent quality.
  • For 4 percent (v/v) acetic acid in aqueous solution, 40 ml of glacial acetic acid is added to water and made up to 1000 ml.
  • For stock solutions, stock solutions containing 1000 mg/liter of lead and at least 500 mg/liter of cadmium, respectively, are prepared in 4 percent acetic acid solution.
• Instruments: The detection limit of the atomic absorption spectrophotometer for lead and cadmium should be equal to or lower than:
  • 0,1 mg/liter for lead
  • 0,01 mg/liter for cadmium

The detection limit is defined as the concentration of the element in 4 percent acetic acid that gives a signal equal to twice the background noise of the instrument.

• Method:
  • Sample preparation: The sample must be clean and free of grease or other substances that could affect the test. The sample is washed in a solution containing household liquid detergent at approximately 40°C. The sample is first rinsed in tap water, then in distilled water or water of equivalent quality. It is drained and dried to avoid any stains. After the surface to be tested has been cleaned, the sample should not be handled.
  • Determination of lead and/or cadmium: The sample prepared in this manner is tested under the conditions specified in the Annex to the Directive (Annex I). Before taking the test solution for the determination of lead and/or cadmium, the content of the sample is homogenized by a suitable method that prevents any loss of solution or corrosion of the tested surface. A blank test is performed on the reagent used for each series of determinations. Determination of lead and/or cadmium is carried out under appropriate conditions by atomic absorption spectrophotometry.

The main objectives of Directive 84/500/EEC are to ensure that ceramic food contact materials do not release harmful levels of lead and cadmium into food, to protect consumer health and to provide a harmonised legal framework across European Union member states.

This directive applies to the following ceramic products:

• Intended to come into contact with foodstuffs
• Already in contact with food
• Which can reasonably be expected to come into contact with food under normal or foreseeable conditions of use.

According to this directive, standardized test methods must be used to determine compliance with migration limits. The simulant used in the migration test method is a 4 percent (v/v) acetic acid solution. This represents acidic foodstuffs and simulates typical contact conditions.

The analytical techniques permitted for the determination of lead and cadmium are:

• Atomic absorption spectrometry (AAS)
• Inductively coupled plasma optical emission spectrometry (ICP-OES)
• Inductively coupled plasma mass spectrometry (ICP-MS)

Other validated methods may also be used as long as they meet the required sensitivity and accuracy.

The directive in question is considered important for the following reasons:

• It helps protect consumer health by limiting exposure to toxic heavy metals.
• It promotes the free movement of goods within the European Union by harmonising rules.
• It provides a legal framework for manufacturers and importers of ceramic food containers.

The amount of lead and cadmium released compared to the specific migration limits defined in the Directive for different ceramic product categories was determined as follows:

• Category 1 Cutlery (e.g. plates): Lead limit 0,8 mg/l, cadmium limit 0,07 mg/l
• Category 2 Hollow containers (e.g. mugs, bowls): Lead limit 4,0 mg/l, cadmium limit 0,3 mg/l
• Category 3 Small containers (e.g. glasses): Lead limit 1,5 mg/l, cadmium limit 0,1 mg/l

Our organization, which has been supporting businesses across all sectors for years through a wide range of testing, measurement, analysis, and evaluation activities, has a strong team of employees who closely follow global developments in science and technology and are constantly improving themselves. In this context, we also provide testing services to businesses within the scope of Directive 84/500/EEC.