EN 16857:2017

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittel - Bestimmung von Benzol in Erfrischungsgetränken, anderen Getränken und in Babynahrung auf Gemüsebasis mit Headspace-Gaschromatographie/Massenspektrometrie (HS-GC-MS)Produits alimentaires - Détermination de la teneur en benzène dans les boissons non alcoolisées, les autres boissons et les aliments pour nourrissons à base de légumes par chromatographie en phase gazeuse avec espace de tête couplée à la spectrométrie de masse (ET CG-SM)Foodstuffs - Determination of benzene in soft drinks, other beverages and vegetable-based infant foods by headspace gas chromatography mass spectrometry (HS-GC-MS)71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysis67.230Predpakirana in pripravljena hranaPrepackaged and prepared foods67.160.20Non-alcoholic beveragesICS:Ta slovenski standard je istoveten z:EN 16857:2017SIST EN 16857:2017en,fr,de01-julij-2017SIST EN 16857:2017SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16857
May
t r s y ICS
x yä s x rä t râ
x yä t u r English Version
Foodstuffs æ Determination of benzene in soft drinksá other beverages and vegetableæbased infant foods by headspace Produits alimentaires æ Détermination de la teneur en benzène dans les boissons non alcooliséesá les autres boissons et les aliments pour nourrissons à base de légumes par chromatographie en phase gazeuse avec
Lebensmittel æ Bestimmung von Benzol in Erfrischungsgetränkená anderen Getränken und in Babynahrung auf Gemüsebasis mit HeadspaceæThis European Standard was approved by CEN on
t r February
t r s yä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
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t r s y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x z w yã t r s y ESIST EN 16857:2017

Typical chromatograms . 13 Annex B (informative)
Precision data . 14 Bibliography . 15
· 99,0 % (CAS 71-43-2). While not necessary, it is recommended to store at 4 °C to 6 °C to prevent evaporation. Bring to room temperature before use. 4.2 Benzene-d6, purity is
· 99, 6 atom % D (CAS 1076-43-3). While not necessary, it is recommended to store at 4 °C to 6 °C to prevent evaporation. Bring to room temperature before use. 4.3 Helium purified compressed gas, purity equivalent to 99,995 % or better. 4.4 Methanol, suitable for headspace GC analysis (CAS 67-56-1). 4.5 Preparation of stock and standard solutions 4.5.1 General Prepare all standard solutions preferably gravimetrically. Record the tare masses of all recipients and the masses after each preparation step and use for calculation of the mass concentrations of standard solutions. SIST EN 16857:2017

approximately 2,20 mg/ml Pipette 20 ml ± 0,1 ml of methanol into a 20 ml headspace vial (5.17) and seal the vial with a crimp cap. Weigh the sealed vial to the nearest 0,1 mg and record the weight as W1. Using a microsyringe, transfer 50 µl of benzene (4.1) through the septum of the vial containing the methanol and shake vigorously or vortex to mix. Reweigh the sealed vial and record the weight (W2) to the nearest 0,1 mg. Subtract W1 from W2 to determine the weight of benzene transferred (W3). Calculate the mass concentration of stock solution from W3 divided by the total volume (20,05 ml). Alternatively, commercially available certified standard solutions may be used if available. Store the benzene stock solution at 4 °C to 6 °C but allow it to attain ambient temperature before use. Discard after 2 weeks. Once the septum on the stock solution has been pierced, the cap shall be replaced. 4.5.3 Benzene intermediate standard solution,
approximately 54 µg/ml Using a microsyringe, transfer 500 µl of benzene stock solution (4.5.2) to a sealed headspace vial containing 20 ml ± 0,1 ml of methanol and shake vigorously. Prepare fresh daily. Calculate the exact mass concentration from the stock solution (4.5.2). 4.5.4 Benzene standard solution,
approximately 0,5 µg/ml Using a microsyringe, transfer 200 µl of benzene intermediate standard solution (4.5.3) to a sealed headspace vial containing 20 ml ± 0,1 ml of water and shake vigorously. Prepare fresh daily. Calculate the exact concentration from the stock solution (4.5.2). Use this standard solution to prepare a 6-point calibration from 0,5 µg/kg to 20 µg/kg (see 4.6). 4.5.5 Benzene-d6 internal standard (IS) stock solution,
approximately 2,36 mg/ml Pipette 20 ml ± 0,1 ml of methanol into a 20 ml headspace vial (5.17) and seal the vial with a crimp cap. Weigh the sealed vial to the nearest 0,1 mg and record the weight as W1. Using a microsyringe, transfer 50 µl of benzene-d6 (4.2) through the septum of the vial containing the methanol and shake vigorously or vortex. Reweigh the sealed vial and record the weight (W2) to the nearest 0,1 mg. Subtract W1 from W2 to determine the weight of benzene-d6 transferred (W3). Calculate the mass concentration of IS stock solution from W3 divided by the total volume (20,05 ml). Alternatively, commercially available certified standard solutions may be used if available. Store the benzene-d6 IS stock solution at 4 °C to 6 °C but allow it to attain ambient temperature before use. Discard after 2 weeks. Once the septum on the IS stock solution has been pierced, the cap shall be replaced. 4.5.6 Benzene-d6 internal standard (IS) solution,
approximately 4,2 µg/ml Using a microsyringe, transfer 36 µl of benzene-d6 IS stock solution (4.5.5) to a sealed headspace vial containing 20 ml ± 0,1 ml of water and shake vigorously. Prepare fresh daily. Calculate the exact mass concentration from the benzene-d6 IS stock solution (4.5.5). 4.6 Preparation of the calibration solutions Prepare calibration solutions of approximately 0 µg/kg, 0,5 µg/kg, 1 µg/kg, 2,5 µg/kg, 5 µg/kg, 10 µg/kg and 20 µg/kg benzene and approximately 10 µg/kg IS according to the following scheme. Add 10 g ± 0,05 g of water to each of seven 20 ml headspace vials and transfer using a positive displacement pipette benzene standard solution (4.5.4), IS solution (4.5.6)and water according to the values given in Table 1. To avoid loss of benzene, seal the vials immediately following addition of the entire benzene and benzene-d6 solutions and water. SIST EN 16857:2017
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