🍎 Lead and cadmium released from ceramic ware — extraction with 4 % acetic acid for 24 h, flame AAS
In short
At least four identical articles are filled with 4 % acetic acid (the simulant) for 24 h, and the lead and the cadmium in the extract are determined by the technique of flame atomic absorption spectrometry; the limits of Directive 84/500/EEC: flatware 0. The test is performed according to PN-EN 1388-1:2000 (+Ap1:2002); Simulant: 4 % acetic acid, contact 24 h. The procedure comprises 7 steps (about 1 days in total); it is used for: Testing of ceramic vessels (plates, mugs, salad bowls, cooking ware) before they are placed on the market — at the request of producers and importers, Official control by the State Sanitary Inspection and risk assessment (RASFF notifications about the migration of metals), Documentation of the declaration of compliance of ceramic articles with Directive 84/500/EEC and with the regulation of the Minister of Health.
At a glance
- Standard: PN-EN 1388-1:2000 (+Ap1:2002)
- Category: Food chemistry
- Procedure steps: 7
- Total time of stages: 1 days
- Simulant: 4 % acetic acid, contact 24 h
- Number of articles in a sample: At least 4 identically decorated ones of an identical or a similar shape
- Technique of measurement: Flame atomic absorption spectrometry (FAAS)
Overview
The standard specifies a method of determining the lead and the cadmium released from ceramic articles intended for contact with food (silicate surfaces); part 2 concerns silicate surfaces other than ceramic ones (for example glass). The text of the standard was not available to us — the description is based on a publication of the National Institute of Public Health – NIH (Bromatologia i Chemia Toksykologiczna 2009), on an article of Łukasiewicz-ICiMB and on the regulations; the laboratory of the National Institute of Public Health carries out the tests in accordance with PN-EN 1388-1:2000 taking into account the regulations of the Minister of Health, using the technique of flame atomic absorption spectrometry, and acts in this field as the national reference laboratory with accreditation to EN ISO/IEC 17025.
Ceramic articles — depending on the quality of the raw materials, the technological process, the kind of food in contact, the time and the temperature of the contact — may release amounts of metals significant for health, chiefly lead and cadmium; the greatest hazard is presented by articles fired at too low a temperature, with a lead glaze, richly decorated on-glaze with a decal with lead and cadmium pigments. In accordance with the regulation of the Minister of Health implementing Directive 84/500/EEC (as amended by Directive 2005/31/EC), the migration of lead and cadmium from flatware must not exceed 0.8 mg/dm² and 0.07 mg/dm² respectively, from hollowware 4.0 mg/l and 0.3 mg/l, and from cooking ware, packaging and storage vessels of a volume above 3 l — 1.5 mg/l and 0.1 mg/l; the standard ISO 6486-2:1999 gives in addition limits for drinking vessels (Pb 0.5 mg/l, Cd 0.25 mg/l). An article meets the requirements if the limits are not exceeded by more than 50 % and the mean of at least three other articles of the same shape, dimensions, decoration and glaze does not exceed the limits.
The simulant is 4 % acetic acid remaining in contact with the vessel for 24 hours — food is chemically less aggressive than the acid used, and the time of contact with a plate is usually shorter; the release of the elements decreases with repeated use and is highest from new articles. In 2007–2008 the laboratory of the National Institute of Public Health tested more than 400 samples of vessels, mostly imported; the majority of the results were below the limit of detection, and 3 samples each of flatware released lead and cadmium above the limits.
Method principle
Every sample consists of at least four identically decorated articles of an identical or a similar shape. The article is filled with the simulant — a 4 % solution of acetic acid — and left in contact for 24 hours (flatware: the surface covered with the simulant, the result referred to a dm²; hollowware: filled to a defined height, the result referred to a litre; drinking vessels in addition the rim — the result in mg per article). The concentration of lead and cadmium in the extract is determined by the technique of flame atomic absorption spectrometry (FAAS) against standard solutions in 4 % acetic acid; the result is calculated as the mass of metal released from a unit of area (mg/dm²) or of volume of simulant (mg/l) and compared with the limits for the given category of article. The details concerning the temperature of the extraction, the lighting, the manner of filling and the criteria of the performance of the analytical method (Directive 2005/31/EC) have to be checked in the text of the standard.
Applications
- Testing of ceramic vessels (plates, mugs, salad bowls, cooking ware) before they are placed on the market — at the request of producers and importers
- Official control by the State Sanitary Inspection and risk assessment (RASFF notifications about the migration of metals)
- Documentation of the declaration of compliance of ceramic articles with Directive 84/500/EEC and with the regulation of the Minister of Health
- Studies of the kinetics of the migration of lead and cadmium from porcelain with repeated extractions
Key parameters
| Parameter | Value |
|---|---|
| Simulant | 4 % acetic acid, contact 24 h |
| Number of articles in a sample | At least 4 identically decorated ones of an identical or a similar shape |
| Technique of measurement | Flame atomic absorption spectrometry (FAAS) |
| Limits — flatware | Pb 0.8 mg/dm², Cd 0.07 mg/dm² |
| Limits — hollowware / cooking and storage ware > 3 l | Pb 4.0 mg/l, Cd 0.3 mg/l / Pb 1.5 mg/l, Cd 0.1 mg/l; drinking vessels according to ISO 6486-2: Pb 0.5 mg/l, Cd 0.25 mg/l |
| Criterion of compliance | An exceedance of the limit of not more than 50 % for a single article, the mean of at least 3 other articles within the limit |
| Presence in accreditation scopes (measured 22.09.2026) | the „Laboratories” tab shows 20 entries at 15 laboratories (matching by the BEGINNING of the string). Those 20 entries are written in EIGHT different ways: „PN-EN 1388-1:2000” (8 entries), „…+Ap1:2002” (4), „…/Ap1:2002” (3), „… + Ap1:2002” (3), „… +Ap1:2002” (2), the number alone without the year (1), „…+ Ap1:2002” (1) and „…+Ap 1:2002” (1). Anyone searching by the exact designation with the amendment will find at most a quarter of the citations |
Standard
- Standard number
- PN-EN 1388-1:2000 (+Ap1:2002)
- Title (PL)
- Materiały i wyroby przeznaczone do kontaktu z produktami spożywczymi — Powierzchnie krzemianowe — Część 1: Oznaczanie ołowiu i kadmu uwalnianego z wyrobów ceramicznych
- Title (EN)
- Materials and articles in contact with foodstuffs — Silicate surfaces — Part 1: Determination of the release of lead and cadmium from ceramic ware
Step-by-step procedure
-
Taking the sample
Assemble at least four identically decorated articles of an identical or a similar shape; classify them into a category (flatware, hollowware, drinking vessels, cooking/storage ware > 3 l).
-
Preparation of the articles
Test new articles in the state as delivered (the greatest release), in accordance with the requirements of the standard as to washing and drying before the test.
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Extraction
Fill the article with 4 % acetic acid (flatware — cover the surface; hollowware — fill to the required height; drinking vessels — in addition the rim), cover it and leave it in contact for 24 h under the conditions laid down in the standard.
-
Measurement
After mixing the extract determine the concentration of Pb and Cd by the technique of flame AAS against a calibration curve in 4 % acetic acid; where necessary dilute the extract with the same acid.
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Calculation
Convert the concentration into mg/dm² of the surface (flatware), mg/l of the simulant (hollowware, drinking vessels, cooking ware) or mg per article (the rim), in accordance with the category of the article.
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Assessment of compliance
Compare with the limits: flatware 0.8 mg Pb/dm² and 0.07 mg Cd/dm²; hollowware 4.0 mg Pb/l and 0.3 mg Cd/l; cooking and storage ware > 3 l 1.5 mg Pb/l and 0.1 mg Cd/l. An article is compliant when the exceedance is not greater than 50 % and the mean of at least three other articles does not exceed the limits.
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Test report
Give the identification of the article (shape, dimensions, decoration, glaze), the category, the conditions of the test, the technique of measurement, the results for every article and the assessment of compliance; for drinking vessels also the result from the rim.
Required equipment and apparatus
| Equipment | Example | Indicative price |
|---|---|---|
| Atomic absorption spectrometer with flame atomisation | Hollow cathode lamps of Pb and Cd, an air–acetylene burner | — |
| The articles tested and covers | At least 4 articles from the sample; a cover limiting evaporation during the 24 h of contact | — |
| Graduated cylinders, pipettes, volumetric flasks | For filling the articles and preparing the standards in 4 % acetic acid | — |
| Measure | For measuring the area covered with the simulant (flatware) and the volume (hollowware) | — |
| Room with a controlled temperature | The extraction under the conditions laid down in the standard | — |
Reagents, media and consumables
| Reagent | CAS | Details |
|---|---|---|
| Acetic acid, solution 4 % | 64-19-7 | The simulant; also for preparing the standard solutions |
| Standard solutions of lead and cadmium | — | Commercial single-element standards, diluted in 4 % acetic acid to the working range of the FAAS |
Health and safety (OHS)
- The extracts contain lead and cadmium — gloves, do not pipette by mouth, the waste as chemical waste
- Acetic acid 4 % — goggles; the vapours from open vessels over 24 h in a ventilated room
- The air–acetylene flame in the AAS — a check of the tightness of the acetylene installation, extraction over the burner
Frequently asked questions
Which standard describes this test?
The test is performed according to PN-EN 1388-1:2000 (+Ap1:2002) — “Materials and articles in contact with foodstuffs — Silicate surfaces — Part 1: Determination of the release of lead and cadmium from ceramic ware”.
How does this method work?
Every sample consists of at least four identically decorated articles of an identical or a similar shape. The article is filled with the simulant — a 4 % solution of acetic acid — and left in contact for 24 hours (flatware: the surface covered with the simulant, the result referred to a dm²; hollowware: filled to a defined height, the result referred to a litre; drinking vessels in addition the rim — the result in mg per article).
What is the measuring range and accuracy?
Simulant: 4 % acetic acid, contact 24 h; Number of articles in a sample: At least 4 identically decorated ones of an identical or a similar shape; Technique of measurement: Flame atomic absorption spectrometry (FAAS); Limits — flatware: Pb 0.8 mg/dm², Cd 0.07 mg/dm².
How long does the test take?
The times given for the individual stages add up to approximately 1 days. The procedure comprises 7 steps.
What equipment is required?
Atomic absorption spectrometer with flame atomisation, The articles tested and covers, Graduated cylinders, pipettes, volumetric flasks, Measure, Room with a controlled temperature.
Where is this test used?
Testing of ceramic vessels (plates, mugs, salad bowls, cooking ware) before they are placed on the market — at the request of producers and importers; Official control by the State Sanitary Inspection and risk assessment (RASFF notifications about the migration of metals); Documentation of the declaration of compliance of ceramic articles with Directive 84/500/EEC and with the regulation of the Minister of Health; Studies of the kinetics of the migration of lead and cadmium from porcelain with repeated extractions.
What safety precautions apply?
The extracts contain lead and cadmium — gloves, do not pipette by mouth, the waste as chemical waste; Acetic acid 4 % — goggles; the vapours from open vessels over 24 h in a ventilated room; The air–acetylene flame in the AAS — a check of the tightness of the acetylene installation, extraction over the burner.
Which laboratory can perform this test?
The test is performed by laboratories accredited to ISO/IEC 17025. On LabCoda you can find them by the standard number PN-EN 1388-1.