1、Foodstuffs - Determination of calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc by ICP-OESBS EN 16943:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16943 May 2017 ICS
2、 67.050 English Version Foodstuffs - Determination of calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc by ICP-OES Produits alimentaires - Dosage du calcium, du cuivre, du fer, du magnsium, du manganse, du phosphore, du potassium, du sodium, du soufre et du
3、zinc par ICP-OES Lebensmittel - Bestimmung von Calcium, Kupfer, Eisen, Magnesium, Mangan, Phosphor, Kalium, Natrium, Schwefel und Zink mit ICP OES This European Standard was approved by CEN on 20 February 2017. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate
4、 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 Stand
5、ard 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 nati
6、onal 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, Ser
7、bia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by
8、 any means reserved worldwide for CEN national Members. Ref. No. EN 16943:2017 ENational forewordThis British Standard is the UK implementation of EN 16943:2017.The UK participation in its preparation was entrusted to Technical Committee AW/275, Food analysis - Horizontal methods.A list of organizat
9、ions represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017 Published by BSI Standards Limited 2017ISB
10、N 978 0 580 91792 9ICS 67.050Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 July 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITIS
11、H STANDARDBS EN 16943:2017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16943 May 2017 ICS 67.050 English Version Foodstuffs - Determination of calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc by ICP-OES Produits alimentaires - Dosage du calcium, du
12、cuivre, du fer, du magnsium, du manganse, du phosphore, du potassium, du sodium, du soufre et du zinc par ICP-OES Lebensmittel - Bestimmung von Calcium, Kupfer, Eisen, Magnesium, Mangan, Phosphor, Kalium, Natrium, Schwefel und Zink mit ICP OES This European Standard was approved by CEN on 20 Februar
13、y 2017. 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 obtai
14、ned 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
15、-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,
16、 Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management
17、 Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16943:2017 EBS EN 16943:2017EN 16943:2017 (E) 2 Contents Page European foreword . 3 1 Scope 4 2 Normative references 4 3 Principle . 4
18、4 Reagents . 5 5 Apparatus . 7 6 Procedure. 8 6.1 Sample preparation 8 6.2 Optical emission spectrometry with inductively coupled plasma 8 6.2.1 ICP-OES working conditions 8 6.2.2 Determination with ICP-OES . 8 6.3 Quality control of the analysis . 10 7 Calculation 10 8 Precision 11 8.1 General . 11
19、 8.2 Repeatability 11 8.3 Reproducibility . 11 9 Test report 14 Annex A (informative) Spectral interferences 15 Annex B (informative) Precision Data . 18 B.1 Details on the inter-laboratory study . 18 Bibliography . 30 BS EN 16943:2017EN 16943:2017 (E) 3 European foreword This document (EN 16943:201
20、7) has been prepared by Technical Committee CEN/TC 275 “Food analysis - Horizontal methods”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2017,
21、 and conflicting national standards shall be withdrawn at the latest by November 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. According to t
22、he CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece,
23、Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16943:2017EN 16943:2017 (E) 4 1 Scope This European Standard describes a method for the
24、 determination of calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc in different foodstuffs using optical emission spectrometry with inductively coupled plasma (ICP-OES) after pressure digestion. This method has been validated in an interlaboratory study acc
25、ording to ISO 5725 1 on infant formula soya based, cheese, chicken meat, wheat flour, apple juice, lobster and milk (see elements ranges Table 1 and validation data in Annex B). HorRat values greater than 2 have been observed for certain analyte/matrix combinations during the validation study. Table
26、 1 Validated element ranges Element Range mg/kg Calcium 70 to 7178 Copper 0,60 to 16,40 Iron 0,88 to 77 Magnesium 45 to 1 174 Manganese 0,44 to 5,12 Phosphorus 72 to 9 708 Potassium 605 to 14 312 Sodium 11 to 2 220 Sulfur 26 to 8 542 Zinc 0,16 to 43,5 At European or International level, vertical sta
27、ndards for the determination of specific minerals can exist, e.g. for milk and milk products or for animal and vegetable fats and oils 2. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For da
28、ted references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 13804, Foodstuffs - Determination of elements and their chemical species - General considerations and specific requirements EN 13805, Foodstuff
29、s - Determination of trace elements - Pressure digestion 3 Principle After digestion of the sample with the pressure digestion process described in EN 13805, calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc are determined quantitatively with the ICP-OES 2.
30、The digestion solution is nebulized, the aerosol is directed into an inductively coupled argon plasma, where the elements are atomized and excited for radiation. The emission radiation is resolved spectrally and its intensity determined at element-specific wavelengths with a detector system. Ionizat
31、ion interference can be minimized using an ionization buffer. BS EN 16943:2017EN 16943:2017 (E) 5 4 Reagents The concentration of the elements to be determined shall be low enough in the reagents and water not to affect the results. 4.1 Nitric acid, minimum w = 65 % 1, density about 1,4 g/ml 4.2 Hyd
32、rochloric acid, w = 30 %, density = 1,15 g/ml 4.3 Hydrogen peroxide, w = 30 % Hydrogen peroxide (4.3) can contain phosphoric acid as a stabilizing agent. Hydrogen peroxide stabilized with phosphoric acid contaminates the samples with phosphorus and thus leads to incorrect results. 4.4 Caesium chlori
33、de solution as ionization buffer, e.g. w = 10 % (see 6.2.2) 4.5 Internal standard, e.g. scandium, ytterbium, yttrium Depending on the matrix, e.g. for samples with high total salt content, the application of an internal standard can be advantageous in order to reduce physical interference. In doing
34、so, it shall be ensured that no faults from line interference result due to the internal standard. NOTE It has been shown that if an internal standard is used, it is applicable to all elements mentioned in the scope. 4.6 Stock solutions, = 1 000 mg/l 2per element Calcium, copper, iron, magnesium, ma
35、nganese, phosphorus, potassium, sodium, sulfur and zinc individual element stock solutions and internal standard used. The individual element stock solutions may not contain any of the elements to be determined here as accompanying substances or impurities, which could affect the correctness of the
36、results. Alternatively, commercial mixed stock solutions can also be used. 4.7 Standard solutions, = 100 mg/l per element Copper, iron, manganese and zinc standard solution, produced by dilution of the respective stock solution (4.6). Pour 10 ml of water into a 50-ml volumetric flask, add 2 ml of ni
37、tric acid (4.1) and mix. After cooling to room temperature, add exactly 5 ml respectively of the copper, iron, manganese and zinc stock solution (4.6) by pipette and fill up with water to the mark. These standard solutions are stable for at least six months. 4.8 Element reference solutions 4.8.1 Gen
38、eral The concentrations of the reference solutions indicated in 4.8.3 to 4.8.6 serve as examples and shall be modified corresponding to the instrument sensitivity, the direction of viewing (axial or radial) and the concentration range to be examined, if necessary. If possible, the calibration shall
39、be performed in the 1w = mass fraction 2 = mass concentration BS EN 16943:2017EN 16943:2017 (E) 6 linear range. Minimum 3, in the nonlinear range 5, reference solutions of different concentrations should be prepared for the calibration. The concentration of the reagents (acids, if applicable ionizat
40、ion buffer and internal standard) shall correspond to the sample measuring solution. For reasons of stability and purity, the phosphorus and sulfur reference solutions should be prepared separately from the multi-element reference solutions of the cations. 4.8.2 Preparation of the flask Pour 10 ml t
41、o 20 ml of water into a 100-ml volumetric flask, add 10 ml of nitric acid (4.1) and 2 ml of hydrochloric acid (4.2) and mix. After cooling to room temperature, add stock (4.6) and standard solutions (4.7) by pipette. If using an ionization buffer, add 10 ml of 10 % caesium chloride solution (4.4). I
42、f using an internal standard (4.5), add the corresponding amount. Alternatively, the ionization buffer and/or the internal standard can be pumped via a Y-piece into the sample flow during the measurement. These reference solutions are stable for a month. The following data under 4.8.3 to 4.8.6 serve
43、 as examples and shall be adapted corresponding to the device sensitivity and the emission wavelength selected, and the direction of viewing (axial or radial), if necessary. 4.8.3 Reference solution 1 Pipette the following amounts of stock solutions (4.6) into the prepared 100-ml volumetric flask (4
44、.8.2): 2,0 ml calcium 3) = 20 mg/l calcium; 1,0 ml magnesium = 10 mg/l magnesium; 2,0 ml potassium = 20 mg/l potassium; 1,0 ml sodium = 10 mg/l sodium; Furthermore, pipette the following amounts of standard solutions (4.7) into the same flask and fill up to the mark with water: 0,50 ml copper = 0,5
45、mg/l copper; 0,50 ml iron = 0,5 mg/l iron; 0,50 ml manganese = 0,5 mg/l manganese; 0,50 ml zinc = 0,5 mg/l zinc. 4.8.4 Reference solution 2 Pipette the following amounts of stock solutions (4.6) into the prepared 100-ml volumetric flask (4.8.2): 10,0 ml calcium = 100 mg/l calcium; 5,0 ml magnesium =
46、 50 mg/l magnesium; 10,0 ml potassium = 100 mg/l potassium; 5,0 ml sodium = 50 mg/l sodium. 3) the sign “ means: “which leads to a mass concentration of“ BS EN 16943:2017EN 16943:2017 (E) 7 Furthermore, pipette the following amounts of standard solutions (4.7) into the same flask and fill up to the
47、mark with water: 2,0 ml copper = 2,0 mg/l copper; 2,0 ml iron = 2,0 mg/l iron; 2,0 ml manganese = 2,0 mg/l manganese; 2,0 ml zinc = 2,0 mg/l zinc. 4.8.5 Reference solution 3 Pipette the following amounts of stock solutions (4.6) into the prepared 100-ml volumetric flask (4.8.2): 20,0 ml calcium = 20
48、0 mg/l calcium; 10,0 ml magnesium = 100 mg/l magnesium; 20,0 ml potassium = 200 mg/l potassium; 10,0 ml sodium = 100 mg/l sodium. Furthermore, pipette the following amounts of standard solutions (4.7) into the same flask and fill up to the mark with water: 5,0 ml copper = 5,0 mg/l copper; 5,0 ml iro
49、n = 5,0 mg/l iron; 5,0 ml manganese = 5,0 mg/l manganese; 5,0 ml zinc = 5,0 mg/l zinc. 4.8.6 Reference solutions phosphorus and sulfur Pipette the following amounts of stock solutions (4.6) into the prepared 100-ml volumetric flask (4.8.2) and fill up to the mark with water: 1,0 ml respectively phosphorus and sulfur = 10,0 mg/l phosphorus and sulfur; 5,0 ml respectively phosphorus and sulfur = 50,0 mg/l p
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