Fertilizers and liming materials - Determination of mercury by vapour generation (VG) after aqua regia dissolution

This European Standard specifies a method for the determination of the content of mercury in
fertilizers !and liming materials" after extraction with aqua regia and the detection of mercury by
vapour generation (VG) coupled to an atomic absorption spectrometer or an inductively coupled
plasma-atomic emission spectrometer. A limit of quantification of 0,01 mg/kg is to be expected.
!NOTE The term fertilizer is used throughout the body of this European Standard and includes
liming materials unless otherwise indicated.

Düngemittel und Kalkdünger - Bestimmung von Quecksilber mit Verdampfungstechnik (VG) nach Königswasseraufschluss

Engrais et amendements minéraux basiques - Détermination du mercure par génération de vapeur (VG) après digestion à l'eau régale

Gnojila in sredstva za apnjenje - Določevanje živega srebra s tehniko hladnih par po raztapljanju v zlatotopki (vključno z dopolnilom A1)

Ta evropski standard določa metodo za določevanje vsebnosti živega srebra v gnojilih in sredstvih za apnjenje po ekstrakciji z zlatotopko in določevanje živega srebra s tehniko hladnih par (VG) z atomskim absorpcijskim spektrometrom ali atomskim emisijskim spektrometrom z induktivno sklopljeno plazmo. Pričakovana je meja kvantifikacije 0,01 mg/kg. OPOMBA: Izraz »gnojilo« se uporablja v celotnem glavnem delu tega evropskega standarda in vključuje sredstva za apnjenje, če ni navedeno drugače.

General Information

Status
Published
Publication Date
07-Nov-2017
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
15-Sep-2017
Due Date
20-Nov-2017
Completion Date
08-Nov-2017

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel und Kalkdünger - Bestimmung von Quecksilber mit Verdampfungstechnik (VG) nach KönigswasseraufschlussEngrais et amendements minéraux basiques - Détermination du mercure par génération de vapeur (VG) après digestion à l'eau régaleFertilizers and liming materials - Determination of mercury by vapour generation (VG) after aqua regia dissolution65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 16320:2013+A1:2017SIST EN 16320:2013+A1:2017en,fr,de01-december-2017SIST EN 16320:2013+A1:2017SLOVENSKI

STANDARDSIST EN 16320:20131DGRPHãþD
SIST EN 16320:2013+A1:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16320:2013+A1
February
t r s y ICS
x wä r z r English Version

Fertilizers and liming materials æ Determination of dissolution Engrais et amendements minéraux basiques æ Détermination du mercure par génération de vapeur

Düngemittel und Kalkdünger æ Bestimmung von Königswasseraufschluss This European Standard was approved by CEN on

t { August
t r s u and includes Amendment
s approved by CEN on
s s December
t r s xä

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

CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä

EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels

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 u t rã t r s u ªA sã t r s y ESIST EN 16320:2013+A1:2017

EN 16320:2013+A1:2017 (E) 2 Contents Page European foreword ....................................................................................................................................................... 3 1 Scope .................................................................................................................................................................... 4 2 Normative references .................................................................................................................................... 4 3 Terms and definitions ................................................................................................................................... 4 4 Principle ............................................................................................................................................................. 4 5 Sampling and sample preparation ............................................................................................................ 4 6 Reagents ............................................................................................................................................................. 5 7 Apparatus ........................................................................................................................................................... 6 8 Procedure........................................................................................................................................................... 7 8.1 General ................................................................................................................................................................ 7 8.2 Preparation of the test solution ................................................................................................................. 7 8.2.1 General ................................................................................................................................................................ 7 8.2.2 Preparation ....................................................................................................................................................... 7 8.3 Preparation of the test solution for the correction of matrix effects by spike recovery ....... 8 8.4 Preparation of the blank test solution .................................................................................................... 8 8.5 Preparation of the calibration solutions ................................................................................................ 8 8.5.1 Calibration solutions for the analysis of mercury ............................................................................... 8 8.5.2 Calibration standards .................................................................................................................................... 9 8.6 Determination of mercury ........................................................................................................................... 9 8.6.1 General ................................................................................................................................................................ 9 8.6.2 Determination by VG-AAS ............................................................................................................................ 9 8.6.3 Spectrometer settings of VG-AAS ............................................................................................................... 9 8.6.4 Determination by VG-ICP-AES ................................................................................................................. 10 9 Calculation and expression of the results ........................................................................................... 11 9.1 External calibration .................................................................................................................................... 11 9.2 Correction for spike recovery .................................................................................................................. 11 9.3 Standard addition method ........................................................................................................................ 12 9.4 Calculation of the element content in the sample ............................................................................ 12 10 Precision .......................................................................................................................................................... 13 10.1 Inter laboratory tests .................................................................................................................................. 13 10.2 Repeatability .................................................................................................................................................. 13 10.3 Reproducibility ............................................................................................................................................. 13 11 Test report ...................................................................................................................................................... 14 Annex A (informative)

Results of the inter-laboratory test ....................................................................... 15 Bibliography ................................................................................................................................................................. 16

SIST EN 16320:2013+A1:2017

EN 16320:2013+A1:2017 (E) 3 European foreword This document (EN 16320:2013+A1:2017) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, 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 August 2017, and conflicting national standards shall be withdrawn at the latest by August 2017. This document includes Amendment 1 approved by CEN on 11 December 2016. This document supersedes !EN 16320:2013". The start and finish of text introduced or altered by amendment is indicated in the text by tags ! ". 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. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. According to the 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, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16320:2013+A1:2017

EN 16320:2013+A1:2017 (E) 4 1 Scope This European Standard specifies a method for the determination of the content of mercury in fertilizers !and liming materials" after extraction with aqua regia and the detection of mercury by vapour generation (VG) coupled to an atomic absorption spectrometer or an inductively coupled plasma-atomic emission spectrometer. A limit of quantification of 0,01 mg/kg is to be expected. !NOTE The term fertilizer is used throughout the body of this European Standard and includes liming materials unless otherwise indicated." 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 1482-2, Fertilizers and liming materials - Sampling and sample preparation - Part 2: Sample preparation EN 12944-1:1999, Fertilizers and liming materials and soil improvers - Vocabulary - Part 1: General terms EN 12944-2:1999, Fertilizers and liming materials and soil improvers - Vocabulary - Part 2: Terms relating to fertilizers !EN 12944-3:2001, Fertilizers and liming materials and soil improvers — Vocabulary — Part 3: Terms relating to liming materials " EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12944-1:1999 and EN 12944-2:1999 and !EN 12944-3:2001"apply. 4 Principle Mercury is extracted from the sample with aqua regia and conventional boiling. The concentration of mercury in the extract is measured by (cold) vapour generation (VG) coupled to a suitable detector, such as an atomic absorption spectrometer (AAS) or an inductively coupled plasma-atomic emission spectrometer (ICP-AES). 5 Sampling and sample preparation Sampling is not part of the method specified in this European Standard. A recommended sampling method is given in EN 1482-1. Sample preparation shall be carried out in accordance with EN 1482-2. SIST EN 16320:2013+A1:2017

EN 16320:2013+A1:2017 (E) 5 6 Reagents Use only reagents of recognized analytical grade. Commercially available stock solutions shall be replaced according to the specifications from the supplier or after one year if prepared in the laboratory from available salts. Standard solutions shall be renewed monthly as a general rule. 6.1 Water, conforming to grade 2 of EN ISO 3696. 6.2 Hydrochloric acid, c(HCl) = 12 mol/l; 37

approximately 1,18 g/ml. 6.3 Nitric acid, c(HNO3) = 16 mol/l; not less than 65 % volume fraction,

approximately 1,42 g/ml. 6.4 Mixed acid solution of 0,8 mol/l nitric acid and 1,8 mol/l hydrochloric acid. Mix 150 ml of hydrochloric acid (6.2) and 50 ml nitric acid (6.3) to 1,0 l of water (6.1). 6.5 Standard stock solution, mercury standard stock solution, e.g.

= 1 000 mg/l. Use suitable stock solutions. Single-element stock solutions with adequate specification stating the acid used and the preparation technique are commercially available. It is recommended to use commercially available standard stock solutions for mercury. 6.6 Working standard solutions. Depending on the scope, different working standard solutions may be necessary. In general, the stability of mercury working standard solutions should be checked. 6.6.1 Working standard solution I,

= 10 mg/l for mercury. Dilute 1,00 ml of the standard stock solution for mercury (6.5) to 100,0 ml with the mixed acid solution (6.4). This solution is used to prepare 200 µg/l mercury working standard solution. 6.6.2 Working standard solution II,

= 200

Dilute 2,00 ml of the 10 mg/l mercury working standard solution I (6.6.1) to 100,0 ml with the mixed acid solution (6.4). This solution is used to prepare spiked test solutions and calibration solutions. 6.7 Reducing agents. 6.7.1 General. Tin(II) chloride or sodium borohydride may be used as the reducing agent, but it is not advisable to use the two reagents alternately. Observe the instructions of the manufacturers of the apparatus. The concentration by mass of the reducing agent solutions may be varied to suit the system, and the relevant information provided by the manufacturer of the apparatus shall be observed. 6.7.2 Tin(II) chloride solution, (SnCl2·2H2O) = 100 g/l. Dissolve 50 g of tin(II) chloride in approximately 100 ml of hydrochloric acid (6.2) in a 500 ml volumetric flask and dilute to the mark. Prepare a fresh solution daily. SIST EN 16320:2013+A1:2017

EN 16320:2013+A1:2017 (E) 6 6.7.3 Sodium borohydride solution, e.g.

= 2 g/l. Dissolve 2 g of sodium hydroxide pellets in water, add 2 g of sodium borohydride and dilute to 1 000 ml with water (6.1). Prepare a fresh solution daily and, when necessary, filter before use. When the analysis procedure is of a longer time, it is recommended to cool the sodium borohydride solution (i.e. with ice around the flask) during its use in the vapour generation ICP-AES or AAS measurement. WARNING — It is essential to observe the safety instructions for working with sodium borohydride. Sodium borohydride forms hydrogen with acids and this can result in an explosive air/hydrogen mixture. A permanent extraction system shall be provided at the point where measurements are carried out. 7 Apparatus 7.1 Common laboratory glassware. 7.2 Analytical balance, capable of weighing to an accuracy of 1 mg. 7.3 Inductively coupled plasma-atomic emission spectrometer, with axial or radial viewing of the plasma and with suitable background correction. The settings of the working conditions (e.g. gas flows, RF or plasma power, sample uptake rate, integration time, number of replicates) shall be optimized according the manufacturer’s instructions. Radial viewing of the plasma may be used if it can be shown that the limit of quantification for mercury is below the required legal limit value. 7.4 Atomic absorption spectrometer, equipped with a heated quartz cuvette or a mercury absorption cell, or optionally with an amalgamation system. 7.5 Vapour generation equipment. 7.5.1 Continuous flow or flow-injection cold-vapour system. 7.5.2 Element-specific lamp for mercury. 7.6 Dilutor. Instrument used for automated volumetric dilutions or other appropriate equipment (e.g. pipettes and volumetric glassware) to perform dilutions. The precision and accuracy of this type of equipment for volumetric dilutions shall be established, and controlled and documented regularly. 7.7 Ash-free filter paper, i.e. Whatman 589/2®1) or equivalent quality.

1) Whatman 589/2® is an example of a suitable product available commercially. This Information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product. Equivalent products may be used if they can be shown to lead to the same results. SIST EN 16320:2013+A1:2017

EN 16320:2013+A1:2017 (E) 7 8 Procedure 8.1 General Calibrations by standard additions with several standards or by matrix matching are very powerful calibration techniques and can be used to accurately correct for matrix effects from easy-ionisable elements (multiplicative matrix effects). Additive matrix effects (i.e. spectral interferences) are not corrected for with standard additions calibration. For matrix matching, additive matrix effects will be corrected for when the added matrix is the cause of the matrix effect. The main drawback of calibration by standard addition with several standards is the requirement for a calibration function for each sample type, which is a time consuming process. For matrix matching, a profound knowledge of the sample matrix is needed, which is not always necessarily available. These two techniques may thus not be practical to use in routine fertilizer laboratories. It is therefore suggested that calibrations are to be performed by means of external calibration and correction of matrix effects by addition of one known spike of a standard solution (spike recovery). The method of external calibration and correction for spike recovery allows for the analysis of fertilizers with unknown matrix composition or with a matrix that cannot be easily imitated synthetically. This calibration technique may not be as precise as calibration by standard additions with several standards but the increased uncertainty is small compared to the total uncertainty of the method, if the total analyte concentration is in the linear working range after the spike and the added spike corresponds to at least a doubling of the analyte concentration. Many matrix errors can be compensated for by this procedure, if they are not additive (e.g. spectral interferences). Aliquots of the sample solution are analysed by the means of external calibration and then one aliquot is spiked with known concentrations of the analytes without changing the matrix of the sample solution. The calculated spike recovery is then used to correct the concentration calculated from the external calibration function. The concentration of the spikes shall be in the linear working range of the analytical detection t

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