Sludge, treated biowaste and soil - Determination of elements using inductively coupled plasma mass spectrometry (ICP-MS)

This European Standard specifies a method for the determination of the following elements in aqua regia or nitric acid digests of sludge, treated biowaste and soil:
Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), cesium (Cs), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), gold (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), lutetium (Lu), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseodymium (Pr), rhenium (Re), rhodium (Rh), rubidium (Rb), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tellurium (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium (Tm), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), ytterbium(Yb), yttrium (Y), zinc (Zn), and zirconium (Zr).
The working range depends on the matrix and the interferences encountered.
The method detection limit of the method is between 0,1 mg/kg dry matter and 2,0 mg/kg dry matter for most elements. The limit of detection will be higher in cases where the determination is likely to be interfered (see Clause 4) or in case of memory effects (see e.g. 8.3 of EN ISO 17294-1:2006).
The method has been validated for the elements given in Table A.1 (sludge), Table A.2 (compost) and Table A.3 (soil). The method is applicable for the other elements listed above, provided the user has verified the applicability.

Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen mittels Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS)

Diese Europäische Norm legt ein Verfahren fest, nach dem in Aufschlusslösungen von Schlamm, behandeltem Bioabfall und Boden nach Königswasser  und Salpetersäureaufschluss die folgenden Elemente bestimmt werden:
Aluminium (Al), Antimon (Sb), Arsen (As), Barium (Ba), Beryllium (Be), Blei (Pb), Bor (B), Cadmium (Cd), Caesium (Cs), Calcium (Ca), Cer (Ce), Chrom (Cr), Dysprosium (Dy), Eisen (Fe), Erbium (Er), Europium (Eu), Gadolinium (Gd), Gallium (Ga), Germanium (Ge), Gold (Au), Hafnium (Hf), Holmium (Ho), Indium (In), Iridium (Ir), Kalium (K), Kobalt (Co), Kupfer (Cu), Lanthan (La), Lithium (Li), Lutetium (Lu), Magnesium (Mg), Mangan (Mn), Molybdän (Mo), Natrium (Na), Neodym (Nd), Nickel (Ni), Palladium (Pd), Phosphor (P), Platin (Pt), Praseodym (Pr), Quecksilber (Hg), Rhenium (Re), Rhodium (Rh), Rubidium (Rb), Ruthenium (Ru), Samarium (Sm), Scandium (Sc), Schwefel (S), Selen (Se), Silber (Ag), Silicium (Si), Strontium (Sr), Tellur (Te), Terbium (Tb), Thallium (Tl), Thorium (Th), Thulium (Tm), Titan (Ti), Uran (U), Vanadium (V), Wolfram (W), Wismut (Bi), Ytterbium (Yb), Yttrium (Y), Zink (Zn), Zinn (Sn) und Zirkonium (Zr).
Der Arbeitsbereich hängt von der Matrix und den zu erwartenden Interferenzen ab.
Die Nachweisgrenze des Verfahrens für die meisten Elemente liegt zwischen 0,1 mg/kg Trockenmasse und 2,0 mg/kg Trockenmasse.
Die Nachweisgrenze wird höher ausfallen, wenn bei der Bestimmung Interferenzen möglich sind (siehe Abschnitt 4), oder Memoryeffekte (Verschleppungseffekte) auftreten (siehe z. B. EN ISO 17294 1:2006, 8.3).
Das Verfahren wurde für die Elemente, die in Tabelle A.1 (Schlamm), Tabelle A.2 (Kompost) und Tabelle A.3 (Boden) aufgeführt sind, validiert. Das Verfahren ist für andere als oben aufgeführte Elemente anwendbar, sofern der Anwender die Anwendbarkeit überprüft hat.

Boues, bio-déchets traités et sols - Détermination des éléments en traces par spectrométrie de masse avec plasma induit par haute fréquence (ICPMS)

La présente Norme européenne spécifie une méthode de détermination des éléments suivants dans des digestats d’eau régale ou d’acide nitrique de boues, de bio-déchets traités et de sols :
Aluminium (Al), antimoine (Sb), arsenic (As), baryum (Ba), béryllium (Be), bismuth (Bi), bore (B), cadmium (Cd), calcium (Ca), cérium (Ce), chrome (Cr), cobalt (Co), cuivre (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), or (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), fer (Fe), lanthane (La), plomb (Pb), lithium (Li), lutécium (Lu), magnésium (Mg), manganèse (Mn), mercure (Hg), molybdène (Mo), néodyme (Nd), nickel (Ni), palladium (Pd), phosphore (P), platine (Pt), potassium (K), praséodyme (Pr), rhénium (Re), rhodium (Rh), rubidium (Rb), ruthénium (Ru), samarium (Sm), scandium (Sc), sélénium (Se), silicium (Si), argent (Ag), sodium (Na), strontium (Sr), soufre (S), tellure (Te), terbium (Tb), thallium (Tl), thulium (Tm), étain (Sn), titane (Ti), tungstène (W), uranium (U), vanadium (V), ytterbium(Yb), yttrium (Y), zinc (Zn) et zirconium (Zr).
L’étendue de mesure dépend de la matrice et des interférences rencontrées.
Les limites de détection de la méthode sont comprises entre 0,1 mg/kg de matière sèche et 2,0 mg/kg de matière sèche pour la plupart des éléments. La limite de détection est plus élevée lorsque la détermination est sujette à des interférences (voir l’Article 4) ou en cas d’effets mémoire (voir 8.3 de l’EN ISO 17294 1:2006, par exemple).
La présente méthode a été validée pour les éléments donnés dans le Tableau A.1 (boues), le Tableau A.2 (compost) et le Tableau A.3 (sols). Cette méthode est applicable pour les autres éléments énumérés ci-dessus, sous réserve que l’utilisateur en ait vérifié l'applicabilité.

Blato, obdelani biološki odpadki in tla - Določevanje elementov z masno spektrometrijo z induktivno sklopljeno plazmo (ICP/MS)

Ta evropski standard določa metodo za določevanje naslednjih elementov v zlatotopki ali izvlečku dušikove kisline blata, obdelanih bioloških odpadkov in tal:
aluminij (Al), antimon (Sb), arzen (As), barij (Ba), berilij (Be), bizmut (Bi), bor (B), kadmij (Cd), kalcij (Ca), cerij (Ce), cezij (Cs), krom (Cr), kobalt (Co), baker (Cu), disprozij (Dy), erbij (Er), evropij (Eu), gadolinij (Gd), galij (Ga), germanij (Ge), zlato (Au), hafnij (Hf), holmij (Ho), indij (In), iridij (Ir), železo (Fe), lantan (La), svinec (Pb), litij (Li), lutecij (Lu), magnezij (Mg), mangan (Mn), živo srebro (Hg), molibden (Mo), neodim (Nd), nikelj (Ni), paladij (Pd), fosfor (P), platina (Pt), kalij (K), prazeodim (Pr), renij (Re), rodij (Rh), rutenij (Ru), samarij (Sm), skandij (Sc), selen (Se), silicij (Si), srebro (Ag), natrij (Na), stroncij (Sr), žveplo (S), telurij (Te), terbij (Tb), talij (Tl), torij (Th), tulij (Tm), kositer (Sn), titan (Ti), volfram (W), uran (U), vanadij (V), iterbij (Yb), itrij (Y), cink (Zn) in cirkonij (Zr).
Delovni razpon je odvisen od matrice in motenj, ki se pojavijo.
Meja detekcije te metode za večino elementov je med 0,1 in 2,0 mg/kg suhe snovi. Meja detekcije bo višja v primerih, ko obstaja možnost motnje določevanja (glej točko 4), ali v primeru spominskih učinkov (glej npr. točko 8.3 standarda EN ISO 17294-1:2006).
Metoda je bila potrjena za elemente v preglednicah A.1 (blato), A.2 (kompost) in A.3 (tla). Metoda se uporablja za druge zgoraj navedene elemente, če uporabnik preveri uporabnost.

General Information

Status
Published
Public Enquiry End Date
03-Jan-2016
Publication Date
13-Mar-2017
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
02-Feb-2017
Due Date
09-Apr-2017
Completion Date
14-Mar-2017

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen mittels Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS)Boues, bio-déchets traités et sols - Détermination des éléments en traces par spectrométrie de masse avec plasma induit par haute fréquence (ICPMS)Sludge, treated biowaste and soil - Determination of elements using inductively coupled plasma mass spectrometry (ICP-MS)71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysis13.080.10Chemical characteristics of soils13.030.20Liquid wastes. SludgeICS:Ta slovenski standard je istoveten z:EN 16171:2016SIST EN 16171:2017en,fr,de01-april-2017SIST EN 16171:2017SLOVENSKI

STANDARDSIST-TS CEN/TS 16171:20131DGRPHãþD
SIST EN 16171:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16171
October
t r s x English Version

Sludgeá treated biowaste and soil æ Determination of elements using inductively coupled plasma mass Bouesá bioædéchets traités et sols æ Détermination des éléments en traces par spectrométrie de masse avec

Schlammá behandelter Bioabfall und Boden æ Bestimmung von Elementen mittels Massenspektrometrie mit induktiv gekoppeltem This European Standard was approved by CEN on

s { March
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 Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey andUnited 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 x CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN

s x s y sã t r s x ESIST EN 16171:2017

EN 16171:2016 (E) 2 Contents Page European foreword ....................................................................................................................................................... 4 Introduction .................................................................................................................................................................... 5 1 Scope .................................................................................................................................................................... 6 2 Normative references .................................................................................................................................... 6 3 Principle ............................................................................................................................................................. 6 4 Interferences .................................................................................................................................................... 7 4.1 General ................................................................................................................................................................ 7 4.2 Spectral interferences ................................................................................................................................... 7 4.2.1 Isobaric elemental interferences .............................................................................................................. 7 4.2.2 Isobaric molecular and doubly-charged ion interferences ............................................................. 7 4.2.3 Non-spectral interferences .......................................................................................................................... 7 5 Reagents ............................................................................................................................................................. 8 6 Apparatus ........................................................................................................................................................ 11 6.1 General requirements ................................................................................................................................ 11 6.2 Mass spectrometer ...................................................................................................................................... 11 6.3 Mass-flow controller ................................................................................................................................... 11 6.4 Nebuliser with variable speed peristaltic pump .............................................................................. 11 6.5 Gas supply ....................................................................................................................................................... 11 6.6 Storage bottles for the stock, standard, calibration and sample solutions. ............................ 12 7 Procedure........................................................................................................................................................ 12 7.1 Test sample solution ................................................................................................................................... 12 7.2 Test solution .................................................................................................................................................. 12 7.3 Instrument set-up ........................................................................................................................................ 12 7.4 Calibration ...................................................................................................................................................... 13 7.4.1 Linear calibration function ....................................................................................................................... 13 7.4.2 Standard addition calibration ................................................................................................................. 13 7.4.3 Determination of correction factors ..................................................................................................... 13 7.4.4 Variable isotope ratio ................................................................................................................................. 13 7.5 Sample measurement ................................................................................................................................. 13 8 Calculation ...................................................................................................................................................... 14 9 Expression of results ................................................................................................................................... 14 10 Performance characteristics .................................................................................................................... 15 10.1 Blank ................................................................................................................................................................. 15 10.2 Calibration check ......................................................................................................................................... 15 10.3 Internal standard response ...................................................................................................................... 15 10.4 Interference ................................................................................................................................................... 15 10.5 Recovery .......................................................................................................................................................... 15 10.6 Performance data ......................................................................................................................................... 16 11 Test report ...................................................................................................................................................... 16 Annex A (informative)

Repeatability and reproducibility data ................................................................. 17 SIST EN 16171:2017

EN 16171:2016 (E) 3 Annex B (informative)

Selected isotopes and spectral interferences for quadrupole ICP-MS instruments .................................................................................................................................................... 24 Bibliography ................................................................................................................................................................. 25

SIST EN 16171:2017

EN 16171:2016 (E) 4 European foreword This document (EN 16171:2016) has been prepared by Technical Committee CEN/TC 444 “Test methods for environmental characterization of solid matrices”, the secretariat of which is held by NEN. 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 April 2017, and conflicting national standards shall be withdrawn at the latest by April 2017. 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 supersedes CEN/TS 16171:2012. The preparation of the previous edition of this analytical method by CEN is based on a mandate by the European Commission (Mandate M/330), which assigned the development of standards on sampling and analytical methods for hygienic and biological parameters as well as inorganic and organic determinants, aiming to make these standards applicable to sludge, treated biowaste and soil as far as this is technically feasible. This document contains the following technical changes in comparison with the previous edition: — repeatability and reproducibility data have been added from a European interlaboratory comparison organized by the German Federal Institute for Materials Research and Testing BAM in 2013 (see Annex A). According to the CEN/CENELEC Internal Regulations, the national standards organizations 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16171:2017

EN 16171:2016 (E) 5 Introduction This European Standard is applicable and validated for several types of matrices as indicated in Table 1 (see Annex A for the results of validation). Table 1 — Matrices for which this European Standard is applicable and validated Matrix Materials used for validation Sludge Municipal sludge Biowaste Compost Soil Soil WARNING — Persons using this European Standard should be familiar with usual laboratory practice. This European Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. IMPORTANT — It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. SIST EN 16171:2017

EN 16171:2016 (E) 6 1 Scope This European Standard specifies a method for the determination of the following elements in aqua regia or nitric acid digests of sludge, treated biowaste and soil: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), cesium (Cs), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), gold (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), lutetium (Lu), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseodymium (Pr), rhenium (Re), rhodium (Rh), rubidium (Rb), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tellurium (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium (Tm), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), ytterbium (Yb), yttrium (Y), zinc (Zn), and zirconium (Zr). The working range depends on the matrix and the interferences encountered. The method detection limit of the method is between 0,1 mg/kg dry matter and 2,0 mg/kg dry matter for most elements. The limit of detection will be higher in cases where the determination is likely to be interfered (see Clause 4) or in case of memory effects (see e.g. EN ISO 17294-1:2006, 8.3). The method has been validated for the elements given in Table A.1 (sludge), Table A.2 (compost) and Table A.3 (soil). The method is applicable for the other elements listed above, provided the user has verified the applicability. 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 15934, Sludge, treated biowaste, soil and waste — Calculation of dry matter fraction after determination of dry residue or water content EN 16173, Sludge, treated biowaste and soil — Digestion of nitric acid soluble fractions of elements EN 16174, Sludge, treated biowaste and soil — Digestion of aqua regia soluble fractions of elements EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696) EN ISO 17294-1:2006, Water quality — Application of inductively coupled plasma mass spectrometry (ICP-MS) — Part 1: General guidelines (ISO 17294-1:2004) 3 Principle Digests of sludge, treated biowaste or soil with nitric acid or aqua regia (see EN 16173 and EN 16174) are analysed by ICP-MS to get a multi-elemental determination of analytes. The method measures ions produced by a radio-frequency inductively coupled plasma. Analyte species originating in the digest solution are nebulised and the resulting aerosol is transported by argon gas into the plasma. The ions produced by the high temperatures of the plasma are entrained in the plasma gas and introduced, by means of an interface, into a mass spectrometer, sorted according to their mass-to-charge ratios and quantified with a detector (e.g. channel electron multiplier). SIST EN 16171:2017

EN 16171:2016 (E) 7 NOTE For the determination of tin only aqua regia extraction applies (EN 16174). 4 Interferences 4.1 General Interferences shall be assessed and valid corrections applied. Interference correction shall include compensation for background ions contributed by the plasma gas, reagents, and constituents of the sample matrix. Detailed information on spectral and non-spectral interferences is given in EN ISO 17294-1:2006, Clause 6. 4.2 Spectral interferences 4.2.1 Isobaric elemental interferences Isobaric elemental interferences are caused by isotopes of different elements of closely matched nominal mass-to-charge ratio and which cannot be separated due to an insufficient resolution of the mass spectrometer in use (e.g. 114Cd and 114Sn). Element interferences from isobars may be corrected by taking into account the influence from the interfering element (see EN ISO 17294-1:2006). The isotopes used for correction shall be free of interference if possible. Correction options are often included in the software supplied with the instrument. Common isobaric interferences are given in Table B.1. 4.2.2 Isobaric molecular and doubly-charged ion interferences Isobaric molecular and doubly-charged ion interferences in ICP-MS are caused by ions consisting of more than one atom or charge, respectively. Examples include 40Ar35Cl+ and 40Ca35Cl+ ion on the 75As signal or 98Mo16O+ ions on the 114Cd+ signal. Natural isotope abundances are available from the literature. The accuracy of correction equations is based upon the constancy of the observed isotopic ratios for the interfering species. Corrections that presume a constant fraction of a molecular ion relative to the "parent" ion have not been found to be reliable, e.g. oxide levels can vary with operating conditions. If a correction for an oxide ion is based upon the ratio of parent-to-oxide ion intensities, this shall be determined by measuring the interference solution just before the sequence is started. The validity of the correction coefficient should be checked at regular intervals within a sequence. Another possibility to remove isobaric molecular interferences is the use of an instrument with collision/reaction cell technology. The use of high resolution ICP-MS allows the resolution of these interferences and additionally double-charged ion interferences. The response of the analyte of interest shall be corrected for the contribution of isobaric molecular and doubly charged interferences if their impact can be higher than three times the detection limit or higher than half the lowest concentration to be reported. More information about the use of correction factors is given in EN ISO 17294-1. 4.2.3 Non-spectral interferences Physical interferences are associated with sample nebulisation and transport processes as well as with ion-transmission efficiencies. Nebulisation and transport processes can be affected if a matrix component causes a change in surface tension or viscosity. Changes in matrix composition can cause SIST EN 16171:2017

EN 16171:2016 (E) 8 significant signal suppression or enhancement. Solids can be deposited on the nebuliser tip of a pneumatic nebuliser and on the cones. It is recommended to keep the level of total dissolved solids below 0,2 % (2 000 mg/l) to minimise deposition of solids in the sample introduction system of the plasma torch. An internal standard can be used to correct for physical interferences if it is carefully matched to the analyte, so that the two elements are similarly affected by matrix changes. Other possibilities to minimise non-spectral interferences are matrix matching, particularly matching of the acid concentration, and standard addition. When intolerable physical interferences are present in a sample, a significant suppression of the internal standard signals (to less than 30 % of the signals in the calibration solution) will be observed. Dilution of the sample (e.g. fivefold) usually eliminates the problem. 5 Reagents For the determination of elements at trace and ultra-trace level, the reagents shall be of adequate purity. The concentration of the analyte or interfering substances in the reagents and the water should be negligible compared to the lowest concentration to be determined. 5.1 Water, grade 1 as specified in EN ISO 3696 for all sample preparations and dilutions. 5.2 Nitric acid, HNO3, (HNO3) = 1,4g/ml, c(HNO3) = 15 mol/l, w(HNO3) = 650 g/kg. 5.3 Hydrochloric acid, HCl, (HCl) = 1,18 g/ml, c(HCl) = 12 mol/l, w(HCl) = 370 g/kg. 5.4 Single-element standard stock solutions Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cs, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, In, Ir, K, La, Li, Lu, Mg, Mn, Mo, Na, Nd, Ni, P, Pb, Pd, Pr, Pt, Rb, Re, Rh, Ru, S, Sb, Sc, Se, Si, Sm, Sn, Sr, Tb, Te, Th, Ti, Tl, Tm, U, V, W, Y, Yb, Zn, Zr, (element) = 1 000 mg/l each. Preferably, nitric acid preservation should be applied in order to minimise interferences by chloropolyatom molecules. Bi, Hf, Hg, Mo, Sn, Sb, Te, W and Zr may need hydrochloric acid for preservation. Both single-element standard stock solutions and multi-element standard stock solutions with adequate specification stating the acid used and the preparation technique are commercially available. These solutions are considered to be stable for more than one year, but in reference to guaranteed stability, the recommendations of the manufacturer should be considered. 5.5 Anion standard stock solutions Cl−,34PO−, 24SO−, (anion) = 1 000 mg/l each. Prepare these solutions from the respective acids. The solutions are commercially available. These solutions are considered to be stable for more than one year, but in reference to guaranteed stability, the recommendations of the manufacturer should be considered. 5.6 Multi-element standard stock solutions Depending on the analytes to be determined, different multi-element standard stock solutions may be necessary. In general, when combining multi-element standard stock solutions, their chemical compatibility and the possible hydrolysis of the components shall be regarded. Care shall be taken to prevent chemical reactions (e.g. precipitation). SIST EN 16171:2017

EN 16171:2016 (E) 9 The multi-element standard stock solutions are considered to be stable for several months if stored in the dark. This does not apply to multi-element standard stock solutions that are prone to hydrolysis, in particular solutions of Bi, Mo, Sn, Sb, Te, W, Hf and Zr. Mercury standard stock solutions can be stabilised by adding 1 mg/l Au in nitric acid (5.2) or by adding hydrochloric acid (5.3) up to 0,6 %. NOTE When Au is to be used as a modifier, it cannot be determined accurately itself in the same analysis run. Multi-element standard stock solutions with more elements are allowed, provided that these solutions are stable. 5.6.1 Multi-element standard stock solution A at the mg/l level may contain the following elements: Ag, Al, As, B, Ba, Be, Bi, Cd, Ce, Co, Cr, Cu, Fe, Hg, Li, Mn, Nd, Ni, Pb, Pr, Sc, Se, Si, Sm, Sr, Te, Th, Ti, Tl, U, V, Zn. Use nitric acid (5.2) for stabilisation of multi-element standard stock solution A. Other elements of interest may be added to the standard stock solution, provided that the resulting multi-element solution is stable. 5.6.2 Multi-element standard stock solution B at the mg/l level may contain the following elements: Mo, Sb, Si, Sn, W, Zr. Use hydrochloric acid (5.3) for stabilisation of multi-element standard stock solution B. Other elements of interest may be added to the standard stock solution, provided that the resulting multi-element solution is stable. 5.6.3 Multi-element standard stock solution C at the mg/l level may contain the following elements: Ca, Mg, Na, K, P, S. Use nitric acid (5.2) for stabilisation of multi-element standard stock solution C. 5.7 Multi-element calibration solutions Prepare in one or more steps calibration solutions at the highest concentration of interest. If more concentration levels are needed prepare those similarly. Add acids (5.2 and/or 5.3) to match the acid concentration of samples closely. If traceability of the values is not established check the validity by comparison with a (traceable) independent standard. Check the stability of the calibration solutions. 5.8 Internal standard solution Internal standards can either be added to every flask or added online. It is essential that the same concentration of internal standard is added to all measurement solutions. The elements In, Lu, Re, Ge and Rh have been found suitable for this purpose. The choice of elements for the internal standard solution depends on the analytical problem. The solution of this/these internal standard(s) should cover the mass range of interest. The internal standards elements shall not be analytes and the concentrations of the selected elements should be negligibly low in the digests of samples. SIST EN 16171:2017

EN 16171:2016 (E) 10 Generally, a suitable final concentration of the internal standard in samples and calibration solutions is 1 µg/l to 50 µg/l (for a high and stable count rate). The use of a collision/reaction cell may require higher concentrations. 5.9 Calibration blank solution Prepare the calibration blank solution by diluting acids (5.2, 5.3) with water (5.1) to the same concentrations as used in the calibration solutions and test solutions. 5.10 Test blank solution The test blank solution shall contain all of the reagents in the same concentrations and shall be handled in the same way throughout the procedure as the samples. The test blank solution contains the same acid concentration in the final solution as the test solution after the digestion method is applied. 5.11 Optimisation solution The optimisation solution is used for mass calibration and for optimisation of the instrumental settings, e.g. adjustment of maximal sensitivity with respect to minimal oxide formation rate and minimal formation of doubly charged ions. It should contain elements covering the total mass range, as well as elements prone to a high oxide formation rate or to the formation of doubly charged ions. The composition of the optimisation solution depends on the elements of interest, instrument and manufacturer's instructions. An optimisation solution containing e.g. Mg, Cu, Rh, In, Ba, La, Ce, U and Pb is suitable. Li, Be and Bi are less suitable because they tend to cause memory effects at higher concentrations. The mass concentrations of the elements used for optimisation should allow count rates of more than 104 counts per second. 5.12 Interference check solution The interference check solutions are used to determine the corresponding factors for the correction equations. High demands are made concerning the purity of the basic reagents due to the high mass concentrations. Interference check solutions shall contain all the interferences of practical relevance given in EN ISO 17294-1, at a concentration level at the same range as expected in the samples (see also 10.4). Leaving out an interfering element according to EN ISO 17294-1 is permitted if it can be demonstrated that its impact is negligible and lasting. In unusual situations, the other interfering elements according to EN ISO 17294-1 shall also be investigated for relevance. EXAMPLE An example of the composition of an interference check solution is: (Ca) = 2 500 mg/l; (Cl−) = 2 000 mg/l; (34PO−) = 500 mg/l and (24SO−) = 500 mg/l and for digests also (C) = 1 000 mg/l; (Fe) = 500 mg/l; (Na) = 500 mg/l and (Al) = 500 mg/l. SIST EN 16171:2017

EN 16171:2016 (E) 11 6 Apparatus 6.1 General requirements The stability of samples, measuring, and calibration solutions depends to a high degree on the container material. The material shall be checked according to the specific purpose. For the determination of elements in a very low concentration range (< 1 µg/kg), glass or polyvinyl chloride (PVC) should not be used. Instead, it is recommended that perfluoroalkoxy alkane (PFA), hexafluoroethene propene (FEP) or quartz containers, cleaned with diluted, high quality nitric acid or hot, concentrated nitric acid in a closed system be used. For the determination of elements in a higher concentration range, containers made from high density polyethylene (HDPE) or polytetrafluoroethene (PTFE) are also suited for the collection of samples. Immediately before use, all containers should be washed thoroughly with diluted nitric acid (e.g. w(HNO3) = 10 %), and then rinsed several times with water (5.1). The limit of detection of most elements is affected by contamination of solutions and this depends predominantly on the cleanliness of laboratory air. The use of piston pipettes is permitted and also enables the preparation of smaller volumes of calibration solutions. The application of dilutors is also allowed. Every charge of pipette tips and single-use plastics vessels shall be tested for impurities. For more detailed information on the instrumentation see EN ISO 17294-1:2006, Clause 5. 6.2 Mass spectrometer A mass spectrometer with inductively coupled plasma (ICP) suitable for multi-element and isotope analysis is required. The spectrometer should be capable of scanning a mass range from 5 m/z (amu) to 240 m/z (amu) with a resolution of at least 1 mr/z peak width at 5 % of peak height (mr = relative mass of an atom species; z = charge number). The instrument may be fitted with a conventional or extended dynamic range detection system. Quadrupole ICP-MS, high-resolution ICP-MS, time-of-flight ICP-MS and collision/reaction cell ICP-MS instrumentation are suitable for measurement. 6.3 Mass-flow controller A mass-flow controller on the nebuliser gas supply is strongly recommended. Mass-flow controllers for the plasma gas and the auxiliary gas are preferred. A cooled spray chamber (cold water or Peltier element) may be beneficial in reducing some types of interferences (e.g. from polyatomic oxide species). 6.4 Nebuliser with variable speed peristaltic pump The speed of the pump shall not be too low and the number of rolls as high as possible to provide a stable signal. 6.5 Gas supply 6.5.1 Argon, Ar, with high purity grade, i.e. > 99,99 %. 6.5.2 Reaction gas, e.g. Helium (He), Hydrogen (H2), Oxygen (O2), ammonia gas (NH3), or methane (

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