DIN EN 15764-2010 Foodstuffs - Determination of trace elements - Determination of tin by flame and graphite furnace atomic absorption spectrometry (FAAS and GFAAS) after pressure d.pdf

1、April 2010 Translation by DIN-Sprachendienst.English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、67.050!$aZn“1625575www.din.deDDIN EN 15764Foodstuffs Determination of trace elements Determination of tin by flame and graphite furnace atomic absorptionspectrometry (FAAS and GFAAS) after pressure digestionEnglish translation of DIN EN 15764:2010-04Lebensmittel Bestimmung von Elementspuren Bestimmu

3、ng von Zinn mit Flammen- und Graphitofen-Atomabsorptionsspektrometrie(FAAS und GFAAS) nach DruckaufschlussEnglische bersetzung von DIN EN 15764:2010-04Produits alimentaires Dosage des lments traces Dosage de ltain par spectromtrie dabsorption atomique flamme (SAAF) etspectromtrie dabsorption atomiqu

4、e four graphite (SAAFG) aprs digestion souspressionTraduction anglaise de DIN EN 15764:2010-04www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 18 pages04.10 DIN EN 15764:2010-04 2 A comma is used as the decimal marker. National foreword

5、This standard has been prepared by Technical Committee CEN/TC 275 “Food analysis Horizontal methods” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural Products Standards Co

6、mmittee), Working Committee NA 057-01-09 AA Elemente und ihre Verbindungen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 National Annex NA (informative) Bibliography DIN ISO 5725-1, Acc

7、uracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement

8、method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15764 December 2009 ICS 67.050 English Version Foodstuffs - Determination of trace elements - Determination of tin by flame and graphite furnace atomic absorption spectrometry (FAAS and GFAAS) after pressure digestion Produits alimentaires

9、- Dosage des lments traces - Dosage de ltain par spectromtrie dabsorption atomique flamme (SAAF) et spectromtrie dabsorption atomique four graphite (SAAFG) aprs digestion sous pression Lebensmittel - Bestimmung von Elementspuren - Atomabsorptionsspektrometrie (FAAS und GFAAS) nach Druckaufschluss Th

10、is European Standard was approved by CEN on 7 November 2009. 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 refer

11、ences concerning such national standards may be obtained on application to the CEN 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

12、into its own language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Lat

13、via, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Bruss

14、els 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15764:2009: EBestimmung von Zinn mit Flammen- und Graphitofen-EN 15764:2009 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents .45 Apparat

15、us and equipment 66 Procedure .77 Evaluations .98 Precision 109 Test report . 11Annex A (informative) Results of the inter-laboratory test 12Bibliography . 16DIN EN 15764:2010-04 EN 15764:2009 (E) 3 Foreword This document (EN 15764:2009) has been prepared by Technical Committee CEN/TC 275 “Food anal

16、ysis - 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 June 2010, and conflicting national standards shall be withdrawn at the latest

17、by June 2010. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standard

18、s organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portu

19、gal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15764:2010-04 EN 15764:2009 (E) 4 1 Scope This European Standard specifies a method for the determination of tin in foodstuffs and canned foods by flame and graphite furnace atomic absorption spectrometry (AA

20、S) after pressurized digestion. The collaborative study included foodstuffs such as carrot puree, tomato puree, pineapple, mixed fruit, white wine, peach powder, tomato powder, powdered beans, powdered fruit yoghurt, fish powder, having mass fractions of tin ranging from 43 mg/kg to 260 mg/kg (Flame

21、-AAS) and from 2,5 mg/kg to 269 mg/kg (Graphite Furnace AAS). 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document

22、(including any amendments) applies. EN 13805, Foodstuffs Determination of trace elements Pressure digestion 3 Principle The sample is mineralized through pressurized digestion with nitric acid and hydrochloric acid in accordance with EN 13805. In the resulting digestion solution, tin is quantified b

23、y flame AAS (F-AAS) or graphite furnace AAS (GF-AAS) depending on the concentration in the sample solution. 4 Reagents 4.1 General The concentration of tin in the reagents and water used shall be low enough not to affect the results of the determination. 4.2 Nitric acid Mass fraction w(HNO3) 65 %, m

24、ass concentration (HNO3) 1,4 g/ml. 4.3 Hydrochloric acid w(HCL) 30 %, (HCl) 1,15 g/ml. 4.4 Tin stock solution (Sn) = 1 000 mg/l. 4.5 Tin standard and calibration solutions 4.5.1 General The standard and calibration solutions are prepared from the stock solution by dilution in glass volumetric flasks

25、. For calibration, prepare at least four calibration solutions of different concentrations. The acid concen-tration shall correspond to the concentration in the measurement solution. DIN EN 15764:2010-04 EN 15764:2009 (E) 5 The preparation of the solutions in 4.5.2 and 4.5.3 is given as an example.

26、4.5.2 Calibration solutions of (Sn) = 5 mg/l, 10 mg/l, 20 mg/l and 30 mg/l for flame AAS. Fill four 50 ml volumetric flasks with 10 ml to 20 ml of water, add 5 ml of nitric acid (4.2) and 1 ml of hydrochloric acid (4.3) and mix. Cool the solutions to ambient temperature, and pipette exactly 0,25 ml,

27、 0,50 ml, 1,00 ml and 1,50 ml of tin stock solution (4.4) for the respective calibration solutions of mass concentrations 5 mg/l, 10 mg/l, 20 mg/l and 30 mg/l into the four different 50 ml volumetric flasks. Mix the solutions and dilute to volume with water. These solutions are stable for at least o

28、ne day. The calibration solutions described here shall be understood as examples. The concentrations prepared shall be in the linear range of the measuring device. The acid concentration of the calibration solutions shall be matched to the acid concentration in the sample solution. 4.5.3 Calibration

29、 solutions of (Sn) = 0,010 mg/l, 0,020 mg/l, 0,040 mg/l and 0,060 mg/l for GF-AAS. To prepare standard solution 1 (Sn) = 50 mg/l), fill a 50 ml volumetric flask with 10 ml to 20 ml of water, add 2,5 ml of hydrochloric acid (4.3) and mix. Cool the solution to ambient temperature, add exactly 2,5 ml o

30、f tin stock solution (4.4) and dilute to volume. This solution is stable for at least one week. To prepare standard solution 2 (Sn) = 1,0 mg/l), fill a 50 ml volumetric flask with 10 ml to 20 ml of water, add 2,5 ml of hydrochloric acid (4.3) and mix. Cool the solution to ambient temperature, add ex

31、actly 1,0 ml of tin standard solution 1 by pipette and dilute to volume. Prepare the calibration solutions for the graphite furnace AAS from standard solution 2 according to the following procedure: Fill four 50 ml volumetric flasks with 10 ml to 20 ml of water, add 5 ml of nitric acid (4.2) and 1 m

32、l of hydro-chloric acid (4.3) and mix. Cool the solutions to ambient temperature, pipette exactly 0,50 ml, 1,0 ml, 2,0 ml and 3,0 ml of standard solution 2 for the respective calibration solutions of mass concentrations 0,010 mg/l, 0,020 mg/l, 0,040 mg/l and 0,060 mg/l into the four different 50 ml

33、volumetric flasks and dilute to final volume with water. These solutions shall be re-prepared for each day of measurement. The calibration solutions described here shall be understood as an example. The concentrations prepared shall be in the linear range of the measuring device. The acid concentrat

34、ion of the calibration solutions shall be matched to the amounts of acid used in the digestion. 4.6 Blank solution The blank solution contains water, nitric acid and hydrochloric acid in amounts that correspond to the concentrations in the measurement solution, for example 10 ml of nitric acid (4.2)

35、 and 2 ml of hydrochloric acid (4.3) in 100 ml of water. 4.7 Matrix modifiers for graphite furnace AAS 4.7.1 General Tin compounds shall be stabilized by matrix modifiers for quantification by graphite furnace AAS during the ashing step. Different matrix modifiers are used at different concentration

36、s. To use a suitable modifier, first consider the recommendations of the device manufacturer. Select a suitable modifier; use the sample matrix to be examined to verify the ashing temperature of the graphite furnace program and optimize it in such a way that no tin is lost in the graphite tube durin

37、g the mineralization step. DIN EN 15764:2010-04 EN 15764:2009 (E) 6 In 4.7.2 to 4.7.4 an example is presented of a modifier for quantifying tin. 4.7.2 Ammonium dihydrogen phosphate solution Mass fraction w 10 %. Dissolve 10,0 g of ammonium dihydrogen phosphate (NH4H2PO4) in 100 ml of water. 4.7.3 Ma

38、gnesium nitrate solution Mass concentration (Mg) = 10 g/l. Dissolve 10,5 g of magnesium nitrate hexahydrate (Mg(NO3)2 6H2O) in 100 ml of water. NOTE Commercially available solutions can also be used. 4.7.4 Matrix modifiers for quantification of tin (NH4H2PO4) = 50 g/10 l and (Mg(NO3)2) = 3 g/10 l. P

39、ipette 2,5 ml of ammonium dihydrogen phosphate solution (4.7.2) and 0,25 ml of magnesium nitrate solution (4.7.3) into a 50 ml volumetric flask; add 1 ml of nitric acid (4.2), and dilute to volume with water. This solution remains usable for several months when refrigerated. 5 Apparatus and equipmen

40、t 5.1 General All apparatus and equipment that come into direct contact with the sample and solutions shall be pre-cleaned appropriately. 5.2 Atomic absorption spectrometer with nitrous oxide/acetylene burner and atomization system. 5.3 Atomic absorption spectrometer with background correction (Zeem

41、ann background correction is recommended), graphite tube furnace and autosampler. 5.4 Element-selective detection 5.4.1 Element-specific lamp for tin (hollow-cathode or electrodeless discharge lamp). 5.4.2 Continuum radiation source with high-resolution monochromatic illuminator as an alternative to

42、 5.4.1. The resolution of the measuring equipment at normal operation shall correspond to at least the half-width value of the emission line of the element specific lamp (usually 1 pm to 3 pm). DIN EN 15764:2010-04 EN 15764:2009 (E) 7 6 Procedure 6.1 Digestion of the sample Mineralize the sample in

43、pressurized digestion in accordance with EN 13805. For the quantification of tin, add 0,5 ml to 1 ml of hydrochloric acid (4.3) to the digestion vessel, which contains nitric acid (4.2) used for the digestion, at an amount that corresponds to the amount of nitric acid. Do not add the hydrochloric ac

44、id until the spontaneous reaction with nitric acid has subsided. After addition of the hydrochloric acid close the digestion vessel immediately in order to avoid loss of active chlorine. Start pressurized digestion shortly thereafter. The digestion requirements are based on the specifications of the

45、 instrument manufacturer, the reactivity of the sample, the maximum pressure stability of the digestion vessel and the attainable temperature. EXAMPLE Precisely weigh 0,4 g to 0,5 g of dry sample (residual moisture of less than 20 %) in a 100 ml digestion vessel and mix it with 5 ml of nitric acid (

46、4.2). Carefully shake the digestion vessel to prevent clots from forming in the sample. After the spontaneous reaction has subsided, add 1 ml of hydrochloric acid (4.3) and close the digestion vessel as quickly as possible. For samples with a higher degree of moisture content, the weighed quantities

47、 can be increased. The digestion solution that results from the pressurized digestion according to EN 13805 can be used directly or can be diluted for the subsequent quantification of tin. 6.2 Flame atomic absorption spectrometry 6.2.1 General Start the instrument and let it stabilise, then optimise

48、 it according to the manufacturers specifications. Set the wavelength to 286,3 nm or 235,5 nm. The nitrous oxide/acetylene flame needs special attention. In general reducing conditions give the best response. If deposits are formed on the burner they need to be removed before they interfere with the

49、 determination. If necessary, use background correction. 6.2.2 Quantification by flame AAS Warm up and stabilize the instrument; then begin measurements. 6.2.3 Calibration and measurement Use the blank solution (4.6) to zero the instrument. Measure the calibration solutions (4.5.2) and use the extinctions (absorbance) and concentrations to generate a calibration curve. Determine the linear range of the calibration function. The measurement solution is taken up and measured.