SIST-TS ISO/TS 16965:2019

TECHNICAL ISO/TS
SPECIFICATION 16965
First edition
2013-09-15
Soil quality — Determination of trace
elements using inductively coupled
plasma mass spectrometry (ICP-MS)
Qualité du sol — Détermination des éléments en traces par spectrométrie
de masse avec plasma induit par haute fréquence (ICP-MS)
Reference number
©
ISO 2013
© ISO 2013
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ii © ISO 2013 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Interferences . 2
4.1 General . 2
4.2 Spectral interferences . 2
5 Reagents . 3
6 Apparatus . 5
6.1 General requirements . 5
6.2 Mass spectrometer . 6
6.3 Mass-flow controller . 6
6.4 Nebuliser with variable speed peristaltic pump . 6
6.5 Gas supply . 6
6.6 Storage bottles, for the stock, standard, calibration and sample solutions . 6
7 Procedure. 7
7.1 Test sample solution . 7
7.2 Test portion solution . 7
7.3 Instrument set up . 7
7.4 Calibration . 8
7.5 Sample measurement . 8
8 Calculation . 9
9 Expression of results . 9
10 Performance characteristics .10
10.1 General .10
10.2 Blank .10
10.3 Calibration check .10
10.4 Internal standard response .10
10.5 Interference .10
10.6 Recovery .10
10.7 Precision .10
11 Test report .11
Annex A (informative) Selected isotopes and spectral interferences for quadrupole ICP-
MS instruments .12
Bibliography .13
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
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electrotechnical standardization.
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described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2. www.iso.org/directives
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to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical
methods and soil characteristics.
iv © ISO 2013 – All rights reserved

Introduction
ISO/TS 16965 is based upon CEN/TS 16171, Sludge, treated biowaste and soil — Determination of elements
using inductively coupled plasma mass spectrometry (ICP-MS), which was developed by CEN/TC 400,
Project Committee — Horizontal standards in the fields of sludge, biowaste and soil.
This Technical Specification is applicable and validated for several types of matrices as indicated in Table 1.
Table 1 — Matrices for which this Technical Specification is applicable and validated
Matrix Materials used for validation
Sludge Municipal sludge
Biowaste Compost
Soil Sludge-amended soils
TECHNICAL SPECIFICATION ISO/TS 16965:2013(E)
Soil quality — Determination of trace elements using
inductively coupled plasma mass spectrometry (ICP-MS)
WARNING — Persons using this Technical Specification should be familiar with usual laboratory
practice. This Technical Specification 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 Technical
Specification be carried out by suitably trained staff.
1 Scope
This Technical Specification specifies a method for the determination of the following elements in aqua
regia or nitric acid digests or other extraction solutions 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 limit of detection 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 have interferences (see
Clause 4) or in the case of memory effects (see e.g. 8.2 of ISO 17294-1:2004).
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.
ISO 11466, Soil quality — Extraction of trace elements soluble in aqua regia
ISO 16729, Soil quality — Digestion of nitric acid soluble fractions of elements
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 17294-1:2004, Water quality — Application of inductively coupled plasma mass spectrometry (ICP-
MS) — Part 1: General guidelines
3 Principle
Digests with nitric acid or aqua regia of samples of sludge, treated biowaste or soil (see ISO 11466 and
ISO 16729) 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
...