EN 16279:2012
(Main)Animal feeding stuffs - Determination of fluoride content after hydrochloric acid treatment by ion-sensitive electrode method (ISE)
Animal feeding stuffs - Determination of fluoride content after hydrochloric acid treatment by ion-sensitive electrode method (ISE)
This European Standard specifies an Ion-Selective Electrode method (ISE) after hydrochloric acid treatment for the determination of fluoride from animal feeding stuffs. The content of fluoride (F-) corresponds to that of fluorine (F) specified in Commission Regulation (EU) 574/2011[3].
This European Standard is strictly based on several conventions such as those contained in the following example:
EXAMPLE 0,5 g test portion for extraction of fluoride from animal feeds by means of an acid treatment with 20 ml of 1 mol/l hydrochloric acid solution at ambient temperature (20 °C to 25 ºC) for 20 min. The pH is controlled and adjusted to 5,5 in the buffered test solution before determination of fluoride by ISE using standard addition technique.
The method was successfully tested in an interlaboratory study in concentrations between 100 mg/kg up to 500 mg/kg. If this method is followed strictly, then theoretically all concentrations from 40 mg/kg up to 4 000 mg/kg can be analysed within the linear calibration function.
Only for concentrations lower than 40 mg/kg is the use of an interpolation technique required instead of standard addition Annex C.
The quantification limit for fluoride using the conventions of the method including the standard addition technique is 40 mg/kg or lower than 2,5 mg/kg when using interpolation Annex C.
Futtermittel - Bestimmung des Fluoridgehaltes nach Salzsäure-Behandlung mit ionensensitiver Elektrode (ISE)
In der vorliegenden Europäischen Norm wird ein Verfahren mit ionenselektiver Elektrode (ISE) zur Bestimmung von Fluorid in Futtermitteln nach Behandlung mit Salzsäure festgelegt. Der ermittelte Fluoridgehalt (F-) entspricht dem Fluorgehalt (F), der in der Verordnung (EG) Nr. 574/2011 der Kommission [3] festgelegt ist.
Diese Europäische Norm beruht streng auf mehreren Konventionen, wie zum Beispiel jene, die im folgenden Beispiel enthalten sind:
BEISPIEL Verwendung einer Prüfmenge von 0,5 g zur Extraktion von Fluorid aus Tierfuttermitteln durch Säurebehandlung mit 20 ml einer Salzsäurelösung (1 mol/l) bei Umgebungstemperatur (20 °C bis 25 °C) für 20 min. Der pH Wert wird kontrolliert und auf 5,5 in der gepufferten Prüflösung vor der Bestimmung von Fluorid mit ISE unter Anwendung des Standardadditionsverfahrens eingestellt.
Das Verfahren wurde erfolgreich in einem Ringversuch mit Konzentrationen von 100 mg/kg bis zu 500 mg/kg geprüft. Wenn die Methodenvorgaben konsequent eingehalten werden, dann können theoretisch alle Konzentrationen von 40 mg/kg bis zu 4 000 mg/kg innerhalb der linearen Kalibrierfunktion analysiert werden.
Nur bei Konzentrationen von weniger als 40 mg/kg ist die Anwendung des Interpolationsverfahrens anstelle des Standardadditionsverfahrens erforderlich (Anhang C).
Unter Berücksichtigung der Konventionen des Verfahrens beträgt die Bestimmungsgrenze mit dem Standardadditionsverfahren 40 mg/kg bzw. weniger als 2,5 mg/kg bei Anwendung des Interpolationsverfahrens (Anhang C).
Aliments des animaux - Détermination de la teneur en fluorure, après traitement à l'acide chlorhydrique, selon la méthode utilisant une électrode sélective d'ions (ISE)
La présente Norme européenne spécifie une méthode utilisant une Electrode Sélective d’Ions (ISE) après traitement à l’acide chlorhydrique pour le dosage du fluorure dans les aliments des animaux. La teneur en fluorure (F-) correspond à celle du fluor (F) tel que spécifié dans le Règlement (UE) n° 574/2011 [3] de la Commission.
La présente Norme européenne repose strictement sur plusieurs conventions telles que celles décrites dans l’exemple suivant :
EXEMPLE l’utilisation d’une prise d’essai de 0,5 g pour l’extraction du fluorure des aliments des animaux par traitement avec 20 ml d’acide chlorhydrique à 1 mol/l à température ambiante (20 °C à 25 °C) pendant 20 min. Le pH est contrôlé et ajusté à 5,5 dans la solution d’essai tamponnée avant le dosage du fluorure par ISE en utilisant la technique des ajouts dosés.
La méthode a passé avec succès un essai interlaboratoires à des concentrations comprises entre 100 mg/kg et 500 mg/kg. En respectant strictement cette méthode, toutes les concentrations comprises entre 40 mg/kg et 4 000 mg/kg peuvent théoriquement être analysées à l’aide de la fonction d’étalonnage linéaire.
Pour les concentrations inférieures à 40 mg/kg uniquement, l’utilisation de la technique d’interpolation à la place de la technique des ajouts dosés est requise (Annexe C).
La limite de quantification pour le fluorure, en utilisant les conventions de la méthode, dont la technique des ajouts dosés, est de 40 mg/kg ou de moins de 2,5 mg/kg avec l’interpolation (Annexe C).
Živalska krma - Določevanje fluorida po obdelavi s solno kislino z metodo ionsko občutljive elektrode (ISE)
Ta evropski standard določa metodo ionsko občutljive elektrode (ISE) po obdelavi s solno kislino za določevanje fluorida v živalski krmi. Vsebnost fluorida (F-) je enaka vsebnosti fluora (F) iz Uredbe Komisije (EU) št. 574/2011. Ta evropski standard strogo upošteva več dogovorov, na primer: preskusni vzorec z maso 0,5 g za ekstrakcijo fluorida iz živalske krme po 20-minutni obdelavi z 20 ml 1 mol/l solne kisline pri temperaturi okolja (20 °C do 25 °C). Vrednost pH pufrske preskusne raztopine se nadzoruje in pred določevanjem fluorida z metodo ionsko občutljive elektrode prilagodi na 5,5 s standardno tehniko dodajanja. Metoda je bila uspešno preskušena v medlaboratorijski študiji pri koncentracijah od 100 mg/kg do 500 mg/kg. Ob natančni uporabi te metode je teoretično možna analiza vseh koncentracij 40 mg/kg do 4 000 mg/kg z linearno funkcijo kalibracije. Tehnika interpolacije se namesto standardnega dodajanja zahteva samo za koncentracije, nižje od 40 mg/kg; glejte dodatek C. Meja kvantifikacije fluorida je ob uporabi dogovorov iz metode, vključno s standardno tehniko dodajanja, 40 mg/kg ali manj kot 2,5 mg/kg, če se uporablja interpolacija; glejte dodatek C.
General Information
Overview
EN 16279:2012 is a CEN European Standard that specifies an Ion-Selective Electrode (ISE) method after hydrochloric acid treatment for the determination of fluoride (F–) in animal feeding stuffs. The measured fluoride content corresponds to fluorine (F) as referenced in Commission Regulation (EU) 574/2011. The method is a potentiometric ISE procedure coupled with a mild HCl extraction intended to reflect gastric conditions and to provide reliable results across a wide concentration range.
Key topics and technical requirements
- Extraction principle: Convention example uses a 0.5 g test portion extracted with 20 ml of 1 mol/l HCl at ambient temperature (20–25 °C) for 20 minutes.
- pH control: After extraction the solution is buffered and adjusted to pH 5.5 ± 0.1 before fluoride measurement.
- Measurement technique: Fluoride is quantified by a fluoride-selective electrode (ISE) using the standard addition technique (with interpolation for very low levels).
- Calibration & working range: The standard describes calibration approaches (recommended working solutions include 0.1, 0.3, 1.0, 3.0 and 10 mg/l) and a linear calibration function that, if conventions are strictly followed, can theoretically cover 40 mg/kg to 4 000 mg/kg.
- Limits of quantification: Using the standard addition conventions, the quantification limit is 40 mg/kg; with interpolation (Annex C) the method can reach below 2.5 mg/kg.
- Validation and precision: The method was validated in an interlaboratory study successfully across 100–500 mg/kg. Precision, sampling and reporting requirements are included.
- Sample preparation: Grinding to specified particle sizes (≤0.5 mm or ≤0.1 mm depending on feed type), and drying procedures for liquid feeds (pre-drying or freeze-drying) are required.
- Safety note: Use appropriate laboratory safety practices for acids and hazardous reagents.
Applications and users
This standard is intended for laboratories and professionals involved in:
- Feed quality control and assurance
- Regulatory compliance and official control testing under EU feed legislation
- Feed manufacturers and ingredient suppliers monitoring fluoride levels
- Animal nutritionists and toxicologists assessing fluoride exposure risk
- Contract testing laboratories offering feed analysis services
Keywords: EN 16279, fluoride determination, ion-selective electrode, ISE method, animal feeding stuffs, feed analysis, hydrochloric acid extraction, fluoride in feed, EU regulation.
Related standards
- EN ISO 3696 - Water for analytical laboratory use
- EN ISO 6498 - Guidelines for sample preparation (animal feeding stuffs)
- EN ISO 6497 - Recommended sampling methods (referenced for sampling)
- Commission Regulation (EU) 574/2011 - Regulatory reference for fluorine content in feeds
This concise guide summarizes the scope and practical use of EN 16279:2012 for laboratories and feed industry stakeholders performing fluoride analysis in animal feeds.
Frequently Asked Questions
EN 16279:2012 is a standard published by the European Committee for Standardization (CEN). Its full title is "Animal feeding stuffs - Determination of fluoride content after hydrochloric acid treatment by ion-sensitive electrode method (ISE)". This standard covers: This European Standard specifies an Ion-Selective Electrode method (ISE) after hydrochloric acid treatment for the determination of fluoride from animal feeding stuffs. The content of fluoride (F-) corresponds to that of fluorine (F) specified in Commission Regulation (EU) 574/2011[3]. This European Standard is strictly based on several conventions such as those contained in the following example: EXAMPLE 0,5 g test portion for extraction of fluoride from animal feeds by means of an acid treatment with 20 ml of 1 mol/l hydrochloric acid solution at ambient temperature (20 °C to 25 ºC) for 20 min. The pH is controlled and adjusted to 5,5 in the buffered test solution before determination of fluoride by ISE using standard addition technique. The method was successfully tested in an interlaboratory study in concentrations between 100 mg/kg up to 500 mg/kg. If this method is followed strictly, then theoretically all concentrations from 40 mg/kg up to 4 000 mg/kg can be analysed within the linear calibration function. Only for concentrations lower than 40 mg/kg is the use of an interpolation technique required instead of standard addition Annex C. The quantification limit for fluoride using the conventions of the method including the standard addition technique is 40 mg/kg or lower than 2,5 mg/kg when using interpolation Annex C.
This European Standard specifies an Ion-Selective Electrode method (ISE) after hydrochloric acid treatment for the determination of fluoride from animal feeding stuffs. The content of fluoride (F-) corresponds to that of fluorine (F) specified in Commission Regulation (EU) 574/2011[3]. This European Standard is strictly based on several conventions such as those contained in the following example: EXAMPLE 0,5 g test portion for extraction of fluoride from animal feeds by means of an acid treatment with 20 ml of 1 mol/l hydrochloric acid solution at ambient temperature (20 °C to 25 ºC) for 20 min. The pH is controlled and adjusted to 5,5 in the buffered test solution before determination of fluoride by ISE using standard addition technique. The method was successfully tested in an interlaboratory study in concentrations between 100 mg/kg up to 500 mg/kg. If this method is followed strictly, then theoretically all concentrations from 40 mg/kg up to 4 000 mg/kg can be analysed within the linear calibration function. Only for concentrations lower than 40 mg/kg is the use of an interpolation technique required instead of standard addition Annex C. The quantification limit for fluoride using the conventions of the method including the standard addition technique is 40 mg/kg or lower than 2,5 mg/kg when using interpolation Annex C.
EN 16279:2012 is classified under the following ICS (International Classification for Standards) categories: 65.120 - Animal feeding stuffs. The ICS classification helps identify the subject area and facilitates finding related standards.
EN 16279:2012 is associated with the following European legislation: EU Directives/Regulations: 70/373/EC; Standardization Mandates: M/382. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Futtermittel - Bestimmung des Fluoridgehaltes nach Salzsäure-Behandlung mittels ISE-VerfahrenAliments des animaux - Détermination de la teneur en fluorure, après traitement à l'acide chlorhydrique, selon la méthode des électrodes sélectives d'ions (ISE)Animal feeding stuffs - Determination of fluoride content after hydrochloric acid treatment by ion-sensitive electrode method (ISE)65.120KrmilaAnimal feeding stuffsICS:Ta slovenski standard je istoveten z:EN 16279:2012SIST EN 16279:2012en,fr,de01-september-2012SIST EN 16279:2012SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16279
July 2012 ICS 65.120 English Version
Animal feeding stuffs - Determination of fluoride content after hydrochloric acid treatment by ion-sensitive electrode method (ISE)
Aliments des animaux - Détermination de la teneur en fluorure, après traitement à l'acide chlorhydrique, selon la méthode utilisant une électrode sélective d'ions (ISE)
Futtermittel - Bestimmung des Fluoridgehaltes nach Salzsäure-Behandlung mit ionensensitiver Elektrode (ISE)This European Standard was approved by CEN on 17 May 2012.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
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Avenue Marnix 17,
B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16279:2012: ESIST EN 16279:2012
Results of the interlaboratory study . 14Annex B (informative)
Flowchart – Determination of fluoride content after hydrochloric acid treatment by ISE method . 15Annex C (informative)
Interpolation reading . 16Bibliography . 18 SIST EN 16279:2012
In particular, fluoride compounds with low solubility are poorly absorbed while fluoride ions released from readily soluble compounds are almost completely absorbed from the gastrointestinal tract by passive diffusion in monogastric species. The extraction procedure of this method involves a mild acid treatment with hydrochloric acid solution of 1 mol/l which should reflect the gastric hydrochloric acid concentration of 0,1 mol/l– 0,3 mol/l.
Specification and test methods EN ISO 6498, Animal feeding stuffs
Guidelines for sample preparation
3 Principle For the determination of fluoride, a test portion of 0,5 g of the sample is treated with 20 ml of 1 mol/l hydrochloric acid solution for 20 min at ambient temperature (20 °C to 25 °C). The amount of fluoride extracted from the sample is determined by means of a fluoride selective electrode. NOTE This ISE method is based upon a potentiometric technique. This means that it is based upon the measurement of a concentration of an analyte present in solution, by means of an ion selective electrode. This electrode has a linear response within a working range of analyte concentrations, which is provided by the calibration curve. Thus, in general, the operator should take an adequate amount of sample to ensure that the final concentration of the analyte is within this working range given by the calibration step. To ensure satisfactory reproducibility of the method however, this extraction procedure as a convention method fixes the ratio of the amount of the test portion to the volume of the extraction solvent for all kind of feeds. WARNING — The use of this European Standard can involve hazardous materials, operations and equipment. This standard does not purport to address all the safety problems associated with its use. It is the responsibility of the user of this European Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. SIST EN 16279:2012
4.3 Hydrochloric acid (HCl), mass fraction of 37 %, having a density of approximately
(HCl) ~ 1,185 g/ml. 4.4 Perchloric acid (HClO4), mass fraction of 70 % to 72 %, having a density of approximately
(HClO4) ~ 1,68 g/ml. 4.5 Acetic acid (CH3COOH), glacial, 99 %.
4.6 Sodium acetate trihydrate (CH3COONa 3H2O), 99 %.
4.7 Trisodium citrate dihydrate (C6H5Na3O7 2H2O), 99 %.
4.8 Hydrochloric acid solution of 1 mol/l.
To prepare: pipette 83 ml hydrochloric acid (4.3) into a 1 000 ml volumetric flask (5.5) and fill to the mark with water (4.1). 4.9 Sodium acetate solution of 3 mol/l.
To prepare: dissolve 408 g of sodium acetate trihydrate (4.6) in 750 ml of water (4.1). When the solution reaches room temperature (20 °C to 25 °C), adjust the pH to 7,0 with acetic acid (4.5), transfer to a 1 000 ml volumetric flask (5.5) and dilute to the mark with water (4.1). 4.10 Sodium citrate solution.
To prepare: dissolve 222 g of trisodium citrate dehydrate (4.7) in 250 ml of water (4.1), add 28 ml perchloric acid (4.4), transfer to a 1 000 ml volumetric flask (5.5) and dilute to the mark with water (4.1). 4.11 Intermediate fluoride solution of 100 mg/l.
To prepare: pipette 10 ml from the 1 000 mg/l fluoride stock solution (4.2) into a 100 ml plastic volumetric flask (5.7) and dilute to the mark with water (4.1). 4.12 Intermediate fluoride solution of 10 mg/l.
To prepare: pipette 10 ml from the 100 mg/l intermediate fluoride solution (4.11) into a 100 ml plastic volumetric flask (5.7) and dilute to the mark with water (4.1). 4.13 Sodium hydroxide solution of 5 mol/l.
To prepare: transfer NaOH pellets, weighing 200 g, to a 1 000 ml volumetric flask (5.5), which is about 2/3 filled with water (4.1) and contains a magnetic stirring bar (5.4). Stir until dissolved; after cooling down take away the magnet stirrer and fill up to the mark with water (4.1) and shake.
NOTE The use of sodium hydroxide solution of 1 mol/l might be more applicable for a precise pH adjustment. SIST EN 16279:2012
5.5 One-mark volumetric flasks, of capacities 100 ml, 500 ml and 1 000 ml. 5.6 Beakers, of capacities 100 ml and 250 ml. 5.7 One-mark plastic volumetric flasks, of capacities 100 ml and 200 ml. 5.8 Plastic beakers, of capacities 50 ml, 100 ml and 200 ml. 5.9 Fluoride selective electrode. NOTE The use of combined electrodes (i.e. selective and reference in one) is possible. 5.10 pH combined electrode. 5.11 Reference electrode for fluoride. 5.12 Ion-pH-meter, capable of measuring to an accuracy of 0,1 mV. 6 Sampling Sampling is not part of the method specified in this European Standard. A recommended sampling method is given in EN ISO 6497 [2]. It is important that the laboratory receives a sample that is truly representative and has not been damaged or changed during transport or storage. 7 Preparation of test sample 7.1 General Prepare the test sample in accordance with EN ISO 6498. The grinding must be performed in conditions such that the substance is not appreciably heated. The operation is to be repeated as many times as is necessary and it shall be executed as quickly as possible in order to prevent any gain or loss of constituents (such as water).
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기사 제목: EN 16279:2012 - 동물 사료 - 염산 처리 후 이온 감지 전극법을 통한 불화물질 함량의 결정 기사 내용: 이 유럽 표준은 동물 사료로부터 불화물질을 결정하기 위한 염산 처리 후 이온 감지 전극법(ISE)을 명시한다. 불화물질(F-)의 함량은 유럽 연합 규정(EU) 574/2011[3]에서 규정된 플루오린(F)의 함량과 일치한다. 이 유럽 표준은 다음 예시에 포함된 것과 같은 여러 가지 협약에 엄격하게 기반을 두고 있다: 예시: 0.5 g의 검사 시료를 1 mol/l 염산 용액 20 ml로 20분 동안 실온(20°C에서 25 ºC)에서 처리하여 동물 사료로부터 불화물을 추출한다. pH는 불화물의 ISE에 의한 결정 전에 5.5로 조절한다. 이 방법은 농도가 100 mg/kg에서 500 mg/kg 사이인 사전 연구에서 성공적으로 테스트되었다. 이 방법이 엄격하게 따라지면 이론적으로는 선형 교정 함수 내에서 40 mg/kg에서 4,000 mg/kg까지의 모든 농도를 분석할 수 있다. 40 mg/kg보다 낮은 농도의 경우에는 표준 첨가 대신 내삽 기법을 사용해야 한다(부록 C). 방법에 따른 불화물의 양적 한계는 표준 첨가 기법을 포함한 방법의 협약에 따라 40 mg/kg 이하이거나 내삽(부록 C)을 사용할 경우 2.5 mg/kg 이하이다.
記事タイトル：EN 16279:2012 - 動物飼料 - 塩酸処理後のイオン感応電極法（ISE）によるフッ化物含有量の決定 記事内容：この欧州標準は、動物飼料からフッ化物含有量を決定するための塩酸処理後のイオン感応電極法（ISE）を指定しています。フッ化物（F-）の含有量は、欧州委員会規則（EU）574/2011[3]で規定されるフッ素（F）の含有量に対応します。 この欧州標準は、以下の例に示すようないくつかの規約に厳密に基づいています: 例：20°Cから25 ºCの室温で、1 mol/lの塩酸溶液20 mlを使用して0.5 gの試験部位からフッ化物を抽出する。フッ化物の決定前に、試験液中のpHを5.5に調整する（バッファ付き試験液を使用）。 この方法は、100 mg/kgから500 mg/kgの範囲での間引き研究で成功裏に検証されました。この方法に厳密に従えば、理論的には線形校正関数内で40 mg/kgから4,000 mg/kgの濃度を分析することができます。 40 mg/kg未満の濃度の場合、標準添加法の代わりに内挿法を使用する必要があります（付録C）。 フルオライドの定量限界は、標準添加法を含む方法の規約に従った場合には40 mg/kg以下、内挿法（付録C）の場合には2.5 mg/kg以下です。
The article discusses EN 16279:2012, a European standard that outlines a method for determining fluoride content in animal feeding stuffs. The method involves treating the sample with hydrochloric acid and using an ion-selective electrode to measure the fluoride content. The standard specifies the extraction process and pH control before conducting the measurement. The method has been successfully tested in various concentrations, and it can analyze fluoride concentrations ranging from 40 mg/kg up to 4,000 mg/kg. For concentrations lower than 40 mg/kg, an interpolation technique is required. The quantification limit for fluoride using the method is 40 mg/kg or lower, depending on the technique used.
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